CN112444753B - Impedance test method for lithium analysis detection of lithium ion battery - Google Patents
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Abstract
The invention belongs to the technical field of lithium ion batteries, and relates to an impedance test method for lithium analysis detection of a lithium ion battery. The conventional characterization method is generally implemented after a large amount of lithium analysis occurs in the battery, and information of a lithium analysis generation node is difficult to obtain. The invention provides an impedance test method, which judges a node where lithium analysis occurs through impedance monitoring by utilizing the principle that the overall impedance of the surface of a negative electrode is reduced when the lithium analysis occurs. The invention applies pulse charging program to the battery, adopts lithium metal as reference electrode to construct a three-electrode battery system, monitors the change of the potential difference of the surface of the negative electrode relative to the reference electrode along with the pulse and relaxation of the battery, and reflects the total impedance of the surface of the negative electrode according to the ratio of the potential difference to the charged current. And observing an inflection point of the total impedance reduced along with the charging depth as a starting point of lithium analysis, and judging whether the lithium analysis action occurs. The invention has simple and quick test process, and can obtain the charging depth when lithium separation occurs under different charging conditions.
Description
Technical Field
The invention belongs to the technical field of lithium ion batteries, and aims to monitor whether lithium analysis behavior of a lithium ion battery occurs or not without disassembling through introducing a reference electrode into the lithium ion battery and monitoring impedance change of a battery cathode so as to prevent excessive lithium analysis of the battery.
Background
With the increasingly shrinking fossil energy and the continuous development of new energy forms, the traditional oil-burning vehicles using petroleum as a power source are gradually transformed into new energy vehicles which are clean and reliable and are driven by electric power. In the new energy automobile, the battery as the power core is the key to realize the transition of the new energy automobile. Due to the stability and long cycle life of the lithium ion battery, the lithium ion battery is generally adopted as an energy source of the new energy automobile at present. However, in recent years, safety accidents of some new energy vehicles are frequent, and the accidents are generally caused by the insecurity of a battery system. In lithium ion batteries, there are many factors causing potential safety hazards, and the lithium precipitation behavior on the surface of a graphite cathode is one of the common inducing factors.
It is generally considered that, when a lithium ion battery is charged at a relatively high current density and a relatively low temperature, lithium ions transferred from the battery positive electrode are precipitated as lithium metal on the surface of the graphite negative electrode. The lithium in the form of metal is precipitated to cause loss of a lithium source, and the lithium metal reacts with an electrolyte to induce heat release and gas generation, which may cause fire explosion of a battery in a serious case. Even if no serious safety problem occurs, lithium metal is separated out to easily form lithium dendrite, and reacts with an electrolyte to form a passivation layer and gradually separates from a current collector to form dead lithium, which also causes the rapid degradation of the battery performance. However, it is also considered that the magnitude of the current applied during the charging process of the battery and the ambient temperature cannot directly determine whether the graphite negative electrode is subjected to lithium precipitation, which makes it difficult to determine whether the lithium precipitation occurs on the surface of the negative electrode during the charging and discharging process of the battery. Therefore, it is important to develop a detection means for determining whether or not lithium analysis has occurred.
However, lithium metal itself has high chemical activity and is easily reacted with various oxidizing substances, and thus, is not suitable for detection in a general atmosphere. In addition, lithium ions are intercalated into graphite to form a lithium-carbon compound, which has similar chemical properties and electrochemical characteristics to metallic lithium, and the two are difficult to distinguish well by some testing means. The current common detection means mainly comprise a scanning electron microscope or a voltage relaxation method. The scanning electron microscope judges whether the precipitation of lithium metal exists or not by observing the difference of the surface appearance of the graphite; the voltage relaxation principle utilizes the principle that precipitated metal lithium is re-embedded into graphite to monitor the voltage change in the process, a differential processing method is adopted to obtain the voltage change rate along with time, and whether the lithium precipitation behavior occurs in the battery process is judged through the occurrence of differential voltage peaks on the curve. Even though the above methods have wide applicability in lithium ion battery research, both of the two detection methods are post-detection methods in the lithium separation process, and the lithium separation behavior of the battery cathode cannot be effectively monitored in real time. Meanwhile, when a scanning electron microscope is used for detection, the battery needs to be disassembled and electrode plates are taken out for sample preparation, so that the integrity of the battery and the subsequent test of the battery are damaged. Therefore, a real-time in-situ and nondestructive means is provided for monitoring the precipitation of lithium metal of the negative electrode of the lithium ion battery, and the method has important significance and necessity for improving the safety and the service life of the battery.
Disclosure of Invention
Technical problem to be solved by the invention
The invention aims to provide an in-situ real-time and nondestructive impedance test means for monitoring lithium analysis behavior of a lithium ion battery cathode. The method has the characteristics of high detection sensitivity, no influence on the normal charging and discharging process of the battery, safe and quick test process and the like, can early warn the lithium analysis behavior of the negative electrode of the battery by analyzing the impedance result, and prevents the potential safety hazard of the battery caused by excessive lithium analysis behavior, thereby realizing the high-safety long-life operation of the battery.
Means for solving the technical problem
In order to solve the above problems, the present invention provides an impedance testing method for lithium analysis detection of a lithium ion battery, which comprises: obtaining the total impedance of the surface of the negative electrode by applying a pulse charging program to the battery; when the total impedance of the surface of the negative electrode is reduced along with the charge deepening, judging as an initial point of lithium separation; and if the battery impedance does not drop or the potential of the negative electrode does not drop below 0V, judging that the lithium precipitation does not occur in the battery.
One embodiment is that, lithium metal is used as a reference electrode in the pulse charging procedure, and the change of the surface potential of the negative electrode in the pulse and relaxation processes is monitored in real time.
In one embodiment, the negative electrode potential is a difference in potential between the negative electrode and a lithium metal reference electrode.
One embodiment is wherein the ratio of the negative electrode surface potential to the applied current density is taken as the total impedance.
One embodiment is, wherein the total negative electrode impedance numerically comprises the interfacial impedance, ohmic impedance, and charge transfer impedance of the negative electrode surface of the lithium ion battery; the interface impedance and the ohmic impedance have no obvious change in the pulse charging process, and the change of the total impedance value of the negative electrode reflects the change of the charge transfer impedance of the negative electrode.
In one embodiment, the node where the charge transfer resistance decreases is the initiation point of lithium deposition; on the trend curve of the overall impedance along with the change of time, the node where the overall impedance value is reduced is the node where the charge transfer impedance is reduced, namely the lithium precipitation occurrence point.
The invention has the advantages of
The invention provides a method for monitoring lithium evolution of a lithium ion battery cathode, which can realize real-time in-situ monitoring, is convenient to use and easy to couple with a battery charging and discharging program, adjusts the charging and discharging program of the battery when a lithium evolution node is judged to occur, and prevents lithium evolution on the surface of the battery cathode, thereby improving the overall safety performance of the battery, hindering active substance loss and interface degradation and prolonging the service life of the battery.
Further features of the present invention will become apparent from the following description of exemplary embodiments.
Drawings
FIG. 1 is a graph of Li-Graphite half-cell voltage versus time and impedance versus time for example 1 in accordance with the present invention;
FIG. 2 is a graph-NCM full-cell voltage time graph and impedance time graph in example 2 of the present invention.
Detailed Description
One embodiment of the present disclosure will be specifically described below, but the present disclosure is not limited thereto.
The conventional characterization method is generally implemented after a large amount of lithium analysis occurs in the battery, and information of a lithium analysis generation node is difficult to obtain. The invention provides an impedance test method, which judges a node where lithium analysis occurs through impedance monitoring by utilizing the principle that the overall impedance of the surface of a negative electrode is reduced when the lithium analysis occurs. The invention applies pulse charging program to the battery, adopts lithium metal as reference electrode to construct a three-electrode battery system, monitors the change of the potential difference of the surface of the negative electrode relative to the reference electrode along with the pulse and relaxation of the battery, and reflects the total impedance of the surface of the negative electrode according to the ratio of the potential difference to the charged current. And observing an inflection point of the total impedance reduced along with the charging depth as a starting point of lithium analysis, and judging whether the lithium analysis action occurs.
In order to achieve the purpose, the invention adopts the following technical scheme:
an impedance test method for lithium analysis detection of a lithium ion battery comprises the following steps:
firstly, assembling a battery needing lithium analysis real-time monitoring according to a three-electrode configuration system, and adopting lithium metal as a reference electrode.
And secondly, performing constant-current pulse charging on the battery by adopting a battery tester, and recording information such as the change of the voltage and the capacity of the battery along with time.
And thirdly, analyzing the voltage-time curve to judge whether the lithium analysis behavior of the graphite cathode of the battery occurs.
The battery test configuration in the step one is simultaneously suitable for a full battery configuration and a half battery configuration, wherein the full battery anode can adopt commercial lithium iron phosphate (LiFePO)4) Lithium cobaltate (LiMn)2O4) Lithium manganate (LiCoO)2) Lithium nickelate (LiNiO)2) And ternary materials, etc., and the negative electrode can adopt artificial graphite, mesocarbon microbeads, hard carbon and other carbon materials, silicon carbon, metal oxide materials, etc. In a half-cell configuration, the working electrode is made of the negative electrode material, and the counter electrode can be made of a lithium metal material.
The electrolyte system adopted in the first step is generally a commercial ester electrolyte.
The reference electrode in the first step adopts a copper wire coated lithium sheet technology, namely, extremely thin metal lithium is wound on the surface of a conductive copper wire, so that the copper wire is completely coated without the surface of the copper wire being exposed, and the lithium-coated part is bent into a ring shape. The other end of the copper wire is used as a current collector to be connected with a measuring instrument, and the middle part of the copper wire is coated by a non-conductive polymer coating layer to prevent the initiation of short circuit of the battery. The reference electrode is isolated from moisture during the manufacturing process.
In the first step, the battery assembly is isolated from water and oxygen, and is carried out under inert conditions, generally in a glove box in an argon atmosphere.
The test instrument used in the second step needs to couple a charging and discharging program and voltage monitoring, and a three-electrode test instrument or two independent channels of a two-electrode test instrument can be adopted.
The pulse charging mode used in the second step can select proper pulse time and relaxation time according to the actual charging rate of the battery.
The analysis method in the third step is based on the principle that the impedance of the negative electrode is suddenly changed by introducing a new electrochemical reaction process when lithium separation occurs. In the normal charging process of the battery, the ohmic impedance of the negative electrode is generally kept unchanged, the interface impedance is stable in the short-time charging and discharging process, and the charge transfer impedance is increased along with the penetration of the lithium embedding process, so that the total impedance of the negative electrode tends to increase continuously. The occurrence of the lithium evolution behaviour introduces a new charge transfer process, resulting in a reduction of the charge transfer resistance, thus causing a reduction of the total resistance. Thus, by detecting the abrupt point of the total impedance during charging, the initial point of occurrence of lithium desorption can be identified. Whether lithium analysis occurs or not is confirmed by analyzing an abrupt fall time node on the impedance-time curve.
The judgment of the lithium analysis behavior in the third step can be verified by means of subsequent optical photos, scanning electron microscopes and the like.
Examples
The present invention is described in more detail by way of examples, but the present invention is not limited to the following examples.
Example 1 determination of lithium evolution behavior of negative electrode in lithium-Graphite (Li-Graphite) half-cell System
(1) Manufacturing a reference electrode: selecting an enameled copper wire with the diameter of 130 mu m, removing polymer coatings with proper lengths at two ends, winding a 30 mu m lithium sheet with a proper length at one end, bending the enameled copper wire into a ring shape after lithium is coated, and not processing the other end;
(2) assembling a Li-Graphite three-electrode half-cell: the graphite cathode adopts mesocarbon microbeads (MCMB), and the weight ratio of MCMB: conductive carbon black (super P): polyvinylidene fluoride (PVDF) ═ 8: 1: the proportion of 1 is that a certain amount of N-methyl pyrrolidone is prepared into slurry and is evenly mixed, the slurry is coated on copper foil by a scraper and then is dried in a blast drier for 24 hours, and a graphite negative electrode circular pole piece with the diameter of 13mm is punched by a punching machine; a16 mm lithium metal pole piece was used for the counter electrode. Reference deviceThe electrodes are placed between the positive and negative electrodes and are separated from the positive and negative electrodes by two PP separators, respectively. The electrolyte adopts 1M lithium hexafluorophosphate (LiPF)6) In an ethylene carbonate/ethyl methyl carbonate mixed solvent (EC/EMC, volume ratio 1: 2). The cell assembly process was performed in a glove box filled with argon.
(3) And (3) testing the battery: the assembled battery is first subjected to three-turn small-rate cyclic activation, the cut-off voltage is set to be 0-1.5V, and the rate is set to be 0.05C (with the theoretical capacity of the graphite cathode as a standard). The multiplying power of the charging process is set to be 2C, and a pulse type charging method with pulse time of 5min and relaxation time of 5min is adopted; the charge curve and the cathode voltage-time curve of the battery were recorded.
(4) And (4) judging lithium analysis behavior: the cell test curve is shown in figure 1. The left graph is a time-varying curve of voltage and current, and an image of the impedance variation with time calculated from the data is shown in the right graph. The impedance is increased along with the increasing charging depth, and meanwhile the potential of the negative electrode is continuously reduced. And (3) as the charging depth continues to deepen, the impedance is suddenly reduced, the potential of the negative electrode is reduced to be below 0V, the lithium precipitation is judged to have occurred in the process, and the lithium intercalation degree is in a range of 70-80%. The dashed curve in the figure represents the potential of the negative electrode after relaxation, which can be approximated as the thermodynamic potential of the negative electrode in this state, which is at a higher level when the impedance curve is abruptly changed, indicating a higher intercalation plateau when actual lithium extraction occurs.
Example 2 lithium evolution behavior in full cells
(1) Manufacturing a reference electrode: selecting an enameled copper wire with the diameter of 130 mu m, removing polymer coatings with proper lengths at two ends, winding a 30 mu m lithium sheet with a proper length at one end, bending the enameled copper wire into a ring shape after lithium is coated, and not processing the other end;
(2) assembling a graphite cathode full battery: selecting ternary material (NCM) as anode material, and coating surface capacity of 2mA h cm-2The positive pole piece is dried in a blast drying oven and then punched into a circular sheet with the diameter of 13 mm. Preparing slurry by the graphite cathode according to the proportion, and then blade-coating the slurry to obtain the surface capacity of 0.6mA h cm-2Drying the negative pole piece in a blast drying ovenThe dried product was punched into a circular piece having a diameter of 13 mm. The reference electrode is placed between the positive and negative electrodes and is separated from the positive and negative electrodes by two PE diaphragms, respectively. The electrolyte adopts 1M lithium hexafluorophosphate (LiPF)6) In an ethylene carbonate/ethyl methyl carbonate mixed solvent (EC/EMC, volume ratio 1: 2). The cell assembly process was performed in a glove box filled with argon.
(3) And (3) full battery test: circulating the Graphite-NCM full battery for 3 circles under the multiplying power of 0.05C (calculated according to the negative electrode capacity) to activate the battery, setting the multiplying power of the charging process to be 2C, and adopting a pulse type charging method with the pulse time of 5min and the relaxation time of 5 min; the charge curve and the cathode voltage-time curve of the battery were recorded.
(4) And (3) lithium separation judgment of the full battery: the full cell test curve is shown in fig. 2. Analysis of the impedance curve shows that lithium precipitation occurs in the full cell at about 80% of the charging depth. By detecting the corresponding relation between lithium analysis behaviors and capacities of batteries with different multiplying powers, the design of the full battery can be guided to prevent lithium analysis.
Industrial applicability
The invention has simple and quick test process, and can obtain the charging depth when lithium separation occurs under different charging conditions.
The present invention is not limited to the above embodiments, and any changes or substitutions that can be easily made by those skilled in the art within the technical scope of the present invention are also within the scope of the present invention. Therefore, the protection scope of the present invention shall be subject to the protection scope of the claims.
Claims (6)
1. An impedance test method for lithium analysis detection of a lithium ion battery comprises the following steps:
charging the battery by applying a pulse charging program to the battery;
calculating the total impedance of the surface of the electrode according to the current in the pulse-relaxation process and the potential change data of the cathode electrode;
when the total impedance of the surface of the negative electrode is reduced along with the charge deepening, judging as an initial point of lithium separation; and if the battery impedance does not drop or the potential of the negative electrode does not drop below 0V, judging that the lithium precipitation does not occur in the battery.
2. The impedance testing method according to claim 1, wherein the change of the negative electrode potential during the pulse and relaxation process is monitored in real time using lithium metal as a reference electrode in the pulse charging procedure.
3. The impedance testing method of claim 1 wherein the negative electrode potential is numerically the negative electrode potential difference from the lithium metal reference electrode.
4. The impedance test method according to claim 1, wherein a ratio of a potential difference of the negative electrode surface potential during pulse-relaxation to an applied current density is taken as a total impedance.
5. The impedance testing method according to claim 1, wherein the negative total impedance numerically comprises an interfacial impedance, an ohmic impedance and a charge transfer impedance of a negative surface of the lithium ion battery; the interface impedance and the ohmic impedance have no obvious change in the pulse charging process, and the change of the total impedance value of the negative electrode reflects the change of the charge transfer impedance of the negative electrode.
6. The impedance testing method according to claim 1, wherein the node at which the charge transfer impedance drops is an initiation point of lithium deposition; on the trend curve of the overall impedance along with the change of time, the node where the overall impedance value is reduced is the node where the charge transfer impedance is reduced, namely the lithium precipitation occurrence point.
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| CN113253122A (en) * | 2021-04-15 | 2021-08-13 | 同济大学 | Rapid lithium analysis detection method for lithium ion battery |
| CN113258156B (en) * | 2021-06-09 | 2021-11-30 | 蜂巢能源科技有限公司 | Three-electrode cell structure, preparation method thereof and method for testing negative electrode potential |
| CN115298561A (en) * | 2021-10-26 | 2022-11-04 | 东莞新能源科技有限公司 | Electrochemical device lithium analysis detection method and system and electrochemical device |
| CN114221049B (en) * | 2021-11-19 | 2023-08-25 | 东莞维科电池有限公司 | Judgment method for lithium precipitation of battery cell |
| CN114200322B (en) * | 2021-12-07 | 2024-04-30 | 欣旺达动力科技股份有限公司 | Lithium ion battery lithium precipitation detection method |
| CN114089202B (en) * | 2022-01-24 | 2022-05-10 | 天津力神电池股份有限公司 | Method for nondestructively analyzing electrode impedance stability in battery circulation process |
| CN114646892B (en) * | 2022-05-19 | 2022-09-27 | 苏州易来科得科技有限公司 | Method and device for obtaining SOC-OCV curve and lithium intercalation-OCV curve of secondary battery |
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