CN112240986A - Lithium precipitation and uniformity evaluation method for large-size soft package lithium ion battery - Google Patents
Lithium precipitation and uniformity evaluation method for large-size soft package lithium ion battery Download PDFInfo
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- G01R31/00—Arrangements for testing electric properties; Arrangements for locating electric faults; Arrangements for electrical testing characterised by what is being tested not provided for elsewhere
- G01R31/36—Arrangements for testing, measuring or monitoring the electrical condition of accumulators or electric batteries, e.g. capacity or state of charge [SoC]
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- G—PHYSICS
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- G01R—MEASURING ELECTRIC VARIABLES; MEASURING MAGNETIC VARIABLES
- G01R31/00—Arrangements for testing electric properties; Arrangements for locating electric faults; Arrangements for electrical testing characterised by what is being tested not provided for elsewhere
- G01R31/36—Arrangements for testing, measuring or monitoring the electrical condition of accumulators or electric batteries, e.g. capacity or state of charge [SoC]
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Abstract
The invention provides a method for evaluating lithium precipitation and uniformity of a large-size soft package lithium ion battery, which comprises the steps of carrying out charge test and discharge test on the lithium ion battery, recording capacity, absolute voltage of the battery, difference value and voltage change condition between an auxiliary lug pair and a main lug, and comparing the time when the voltage reaches a stable state at different positions with the dV/dT curve and the dV/dQ curve obtained by processing; and judging the rate distribution and the lithium precipitation amount of the lithium ions inserted into the graphite according to the dV/dT curve and the dV/dQ curve. The method is simple in operation method, does not damage the battery, is accurate and reliable in data, realizes real-time analysis on lithium precipitation uniformity of the negative electrode in the lithium ion battery, and can provide key technical support for design of soft package single batteries and modules and estimation of the actual service life of the battery pack.
Description
Technical Field
The embodiment of the invention relates to the technical field of lithium ion batteries, in particular to a method for evaluating lithium precipitation and uniformity of a large-size soft package lithium ion battery.
Background
Lithium ion batteries have received more and more attention in recent years as a novel green energy source, and with the continuous expansion of the application range of lithium ion batteries, the requirements for the application conditions of the lithium ion batteries are more and more strict, and what must be solved in the lithium battery industry is how to improve the cycle performance and the high-rate charging performance of the lithium batteries at low temperature. The cathode material of the commercial lithium ion battery comprises carbon, silicon-based materials and the like, because the reaction potential is close to the deposition potential of metal lithium, when the battery is charged at a high rate, at a low temperature or overcharged, the lithium intercalation space of the cathode is insufficient or the lithium intercalation resistance is overlarge, so that lithium precipitation and lithium dendrite formation can occur on the surface of the cathode, and the safety problems of battery capacity reduction, service life attenuation, short circuit and the like are caused. Therefore, the detection and analysis of lithium ions in lithium ion batteries have become a technical hotspot in the industry at present.
The patent with application number 201810769863.3 proposes a method for determining lithium ion battery lithium-separation critical conditions, which comprises charging at different rates at the same temperature, and recording the relationship between the negative electrode potential and the charging current or charging rate to obtain the lithium ion battery critical lithium-separation or critical lithium-separation rate. The patent with the application number of 201810576440.X provides a lithium analysis detection method and system for a lithium ion battery, differentiation processing is carried out on charging voltage and capacity data of the lithium ion battery to obtain a dV/dQ curve, and a lithium analysis state inside the lithium ion battery is judged. Patent application No. 201610367810.X proposes a method for comparing coulombic efficiency data of charge-discharge cycles before and after standing of a lithium ion battery to directly determine whether lithium precipitation occurs in the lithium ion battery.
The technical scheme is only related analysis performed after lithium is separated from the lithium ion battery cathode, accurate test on the nonuniform distribution of lithium separated from the lithium ion battery cannot be performed, the design size of the lithium ion battery is required to be continuously increased in the power lithium ion battery market, and the prior technical scheme cannot provide related technical support and meet the latest market demand.
Disclosure of Invention
The invention provides a method for evaluating lithium separation and uniformity of a large-size soft package lithium ion battery, aiming at solving the problem that the lithium separation non-uniform distribution in the lithium ion battery cannot be accurately tested, and the method is constructed.
In order to achieve the above purpose, the present invention provides the following technical solutions:
a method for evaluating lithium precipitation and uniformity of a large-size soft package lithium ion battery comprises the following steps:
step S1: carrying out charge test and discharge test on the lithium ion battery, and recording the capacity, the absolute voltage of the battery, the difference between the auxiliary lug pair and the main lug and the voltage change condition;
step S2: comparing the time when the voltage reaches the steady state at different positions, and drawing a dV/dT curve by taking the time T as an X axis and the dV/dT as a Y axis;
step S3: performing differential processing on the dV/dT curve, and then drawing by taking the discharge capacity Q as an X axis and the dV/dQ as a Y axis to obtain a dV/dQ curve;
step S4: and judging the rate distribution and the lithium precipitation amount of the lithium ion intercalated graphite by taking the discharge capacity Q as an X axis and the dV/dQ as a Y axis according to the dV/dT curve and the dV/dQ curve.
After the lithium ion battery is charged and discharged at a large current, the duration of voltage stabilization depends on the rate capability of lithium ions to be embedded into graphite, parameters such as the exchange current density of intercalation, the solid diffusivity of graphite, temperature and the like, and even under the condition that the lithium metal content is the same, the voltage curve can be obviously influenced. Therefore, the method of comparing the lithium plating amount of different positions of the battery by using the voltage plateau period under a certain constant temperature by using the same battery pack is reasonable.
The step of carrying out the charging test on the soft package lithium ion battery comprises the following steps:
step 101: treating the soft package lithium ion battery at low temperature;
step 102: charging to a specified electric quantity by constant current, and keeping an open circuit for a period of time;
step 103: and observing and recording the capacity, the absolute voltage of the battery, the difference between the auxiliary pole lug pair and the main pole lug and the voltage change condition.
The step of carrying out discharge test on the soft package lithium ion battery comprises the following steps:
step 111: the soft package lithium ion battery is processed at a low temperature;
step 112: discharging immediately after charging to a specified electric quantity with a constant current;
step 113: and observing and recording the capacity, the absolute voltage of the battery, the difference between the auxiliary pole lug pair and the main pole lug and the voltage change condition.
The step of judging the rate distribution of lithium ion intercalation into graphite and the amount of lithium precipitation includes:
step 401: according to the dV/dT curve, the X axis is time, the Y axis is dV/dT, any X coordinate is taken as a perpendicular line and is intersected with a corresponding point of the dV/dT curve to obtain an intersection point; making a tangent line of the dV/dT curve through the intersection point, solving the slope of the tangent line, namely the rate of lithium ions embedded into the graphite, and measuring the rate corresponding to the needed X coordinate for multiple times to obtain the rate distribution of the lithium ions embedded into the graphite;
step 402: according to the dV/dQ curve, making any X bid to make a vertical line to intersect with a corresponding point of the curve to obtain an intersection point; crossing the crossing point with a horizontal line and crossing the Y axis to obtain a point crossing the Y axis, and calculating the mass of the precipitated lithium according to the formula that m lithium (g) = Q × 3600 × 6.94/96500 by taking the capacity corresponding to the point crossing the Y axis.
Preferably, during the discharge, the discharge current is in the range of 0.3-1.0C and the cut-off voltage is 2.7V.
Preferably, the temperature range of the low-temperature environment is-10 ℃ to 5 ℃, and the temperature value and the current value selected in the charging test step and the discharging test step are kept consistent.
Preferably, the tab difference between the auxiliary tab and the main tab is measured by a high-precision analog data recorder.
The invention researches relaxation behaviors of different multiplying power charge and discharge of the battery at low temperature by independently designing a multi-tab soft package battery and adopting a high-precision analog data recorder. And comparing the voltage stabilization time and the dV/dT and dV/dQ curves at different positions, the rate distribution and the lithium precipitation amount of lithium ion-intercalated graphite can be visually obtained, and the influence of the battery size on the local uniformity of the battery can be obtained. The method is simple in operation method, does not damage the battery, is accurate and reliable in data, realizes real-time analysis on lithium precipitation uniformity of the negative electrode in the lithium ion battery, and can provide key technical support for design of soft package single batteries and modules and estimation of the actual service life of the battery pack.
Drawings
FIG. 1 is a schematic diagram of a multi-tab large-size soft-package lithium ion battery;
wherein: 1. battery core main lug 2, auxiliary lug pair 3 and temperature probe
Fig. 2 is a schematic flow chart of a detection method for lithium separation of a soft package lithium ion battery.
FIG. 3 is a lithium analysis quality meter for different locations charging process
FIG. 4 is a time chart of voltage equilibrium at different positions of the discharge process
FIG. 5 is a time chart of the voltage reaching equilibrium at different positions during the charging process
FIG. 6 is a dV-dT diagram of the discharge process
FIG. 7 is a dV-dT diagram of a charging process
Fig. 8 is a dV/dQ diagram of the discharge process of a multi-tab battery at different positions (the embedded part is a partially enlarged view).
Detailed Description
Example (b): a method for evaluating lithium separation and uniformity of a large-size soft package lithium ion battery is suitable for a multi-tab large-size soft package lithium ion battery, please refer to the attached drawing 1, which is a schematic diagram of the multi-tab large-size soft package lithium ion battery, the multi-tab large-size soft package lithium ion battery comprises a battery main body, a main battery cell tab and an auxiliary tab pair, wherein the main battery cell tab is positioned on the same side; the auxiliary lug pairs are symmetrically distributed on two sides of the length of the battery, the interval between adjacent auxiliary lugs is equal, the main body of the battery comprises a positive pole piece and a negative pole piece, the positive pole piece is made of layered transition metal oxide, the negative pole piece is made of silicon-based material, 6 temperature probes are arranged in the main body, and the temperature probes are positioned in the middle of the auxiliary lug pairs.
The auxiliary pole lugs are symmetrically distributed at equal intervals and are respectively numbered as 1#, 2#, 3#, 4#, 5# and 6#, the positions to be measured can be arranged in an array mode, certain rules are provided, analysis of measured data is facilitated, and therefore the analysis result is more accurate.
The auxiliary lug pair is located at the detected position, the temperature probe is located in the middle of the auxiliary lug pair, and the temperature measured by the temperature probe can reflect the temperature of the auxiliary lug pair at the detected position and can be synchronously processed with other parameters such as voltage, capacity and the like.
Please refer to fig. 2, which is a schematic flow chart of a detection method for lithium separation of a soft package lithium ion battery, and is an evaluation method for lithium separation and uniformity of a large-size soft package lithium ion battery, wherein a charging test and a discharging test are performed on the lithium ion battery, the capacity, the absolute voltage of the battery, the difference between an auxiliary tab pair and a main tab pair and the voltage change condition are recorded, the time when the voltage reaches a steady state at different positions is compared, and a dV/dT curve is obtained by plotting with the time T as an X axis and dV/dT as a Y axis; carrying out differential processing on the dV/dT curve, and drawing by taking the discharge capacity Q as an X axis and the dV/dQ as a Y axis to obtain a dV/dQ curve; and judging the rate distribution and the lithium precipitation amount of the lithium ions inserted into the graphite according to the dV/dT curve and the dV/dQ curve. After the lithium ion battery is charged and discharged at a large current, the duration of voltage stabilization depends on the rate capability of lithium ions to be embedded into graphite, parameters such as the exchange current density of intercalation, the solid diffusivity of graphite, temperature and the like, and even under the condition that the lithium metal content is the same, the voltage curve can be obviously influenced. Therefore, the method of comparing the lithium plating amount of different positions of the battery by using the voltage plateau period under a certain constant temperature by using the same battery pack is reasonable.
The step of carrying out the charging test on the soft package lithium ion battery comprises the following steps:
step 101: the soft package lithium ion battery is placed in a low-temperature environment of-10 ℃ for 4 hours;
step 102: charging to 75% SOC at constant current 3C, keeping open circuit for 3 hours;
step 103: the capacity and the absolute voltage of the battery are observed and recorded, and the auxiliary pole difference value and the voltage change are measured by using a high-precision analog data recorder.
The step of carrying out discharge test on the soft package lithium ion battery comprises the following steps:
step 111: the soft package lithium ion battery is placed in a low-temperature environment of-10 ℃ for 4 hours, the low-temperature environment and the processing time are consistent when the charging test is carried out, the low-temperature environment and the processing time are comparable under the same condition, and the two groups of data can be merged and compared;
step 112: discharging immediately after charging to 75% SOC at a constant current of 3C, wherein the discharging current is 0.3C, and the cut-off voltage is 2.7V;
step 113: the capacity and the absolute voltage of the battery are observed and recorded, and the auxiliary pole difference value and the voltage change are measured by using a high-precision analog data recorder.
The step of judging the rate distribution of lithium ion intercalation into graphite and the amount of lithium precipitation includes:
comparing the time when the voltage reaches the steady state at different positions with the dV/dT curve obtained by processing, processing the data recorded in the discharging process to obtain a dV/dQ curve, wherein the dV/dQ curve is obtained by firstly differentiating the discharging curve, and then drawing by taking the discharging capacity Q as an X axis and the dV/dQ as a Y axis, so that the dV/dQ curve can be obtained, as shown in FIG. 8. And intuitively obtaining the rate distribution of lithium ions inserted into the graphite according to the dV/dT curve, and estimating the Li precipitation amount at different positions according to the dV/dQ curve.
In combination with comparing fig. 4-7, it can be seen that the voltage reaches different stabilization times in the charge relaxation phase at different positions, which is related to the lithium deposition rate at different positions, and the voltage is stabilized faster the lithium deposition rate is. But because all positions have reached a steady state in a short time, the dV/dT plots at the different positions are very close.
The voltage plateau of the discharge curve of a lithium ion battery represents the phase transition process in the electrode, and since the oxidation reaction, i.e. the delithiation process, occurs on the negative electrode during the discharge process, the oxidation reaction comprises the extraction of lithium embedded inside the negative electrode and the oxidation of surface lithium deposition, wherein the surface lithium deposition is generated in the previous charging process and preferentially reacts during the delithiation process, the high voltage plateau of the discharge curve represents the oxidation reaction of lithium deposition on the surface of the negative electrode, which is caused by the phase equilibrium between the surface lithium deposition and the first delithiation stage of graphite. In the invention, a low-temperature test environment is adopted, so that the side reaction of lithium film deposition on the surface can be ignored, and the capacity Q (mAh) corresponding to the dV/dQ peak position of a discharge curve is caused by the complete oxidation reaction of the lithium deposition on the surface, and then according to a formula:
m lithium (g) = Q3600 x 6.94/96500
The mass of precipitated lithium can be calculated. The specific calculation result is shown in fig. 3 and the lithium analysis quality table in the charging process at different positions, and it can be seen that in the same test step, the lithium analysis quality at different positions of the same battery pack is obviously different, which is related to the kinetic process of the lithium analysis reaction at different positions. Comparing the time when the voltage at different positions reaches a stable state with the dV/dT curve obtained by processing, wherein the dV/dT curve has the X axis as time and the Y axis as dV/dT, and any X coordinate is crossed with the corresponding point of the dV/dT curve by drawing a vertical line to obtain an intersection point; making a tangent line of the dV/dT curve through the intersection point, solving the slope of the tangent line, namely the rate of lithium ions embedded into the graphite, and measuring the rate corresponding to the needed X coordinate for multiple times to obtain the rate distribution of the lithium ions embedded into the graphite; the effect of cell size on the local uniformity of the cell was analyzed. The data recorded during the discharge process is processed to obtain a dV/dQ curve, and the discharge capacity of the peak of the dV/dQ curve can be approximately equal to the amount of lithium deposited during the charge process, and can be used for estimating the amount of lithium deposited at different positions.
The embodiment of the invention provides a multi-tab large-size lithium ion soft package battery which is used for testing relaxation behaviors of different-rate charge and discharge of the battery at low temperature. And comparing the voltage stabilization time and the dV/dT and dV/dQ curves at different positions, the rate distribution and the lithium precipitation amount of lithium ion-embedded graphite can be visually obtained, and the influence of the size of the battery on the local uniformity of the battery can be obtained on the premise of not damaging the battery.
The invention utilizes the independently designed multi-tab soft package battery, adopts the high-precision analog data recorder to research the relaxation behavior of the low-temperature battery, has simple operation method, no damage to the battery and accurate and reliable data, realizes the real-time analysis of the lithium precipitation uniformity of the negative electrode in the lithium ion battery, and can provide key technical support for the design of the soft package single battery and the module and the estimation of the actual service life of the battery pack.
Claims (8)
1. A method for evaluating lithium precipitation and uniformity of a large-size soft package lithium ion battery is characterized by comprising the following steps:
step S1: carrying out charge test and discharge test on the lithium ion battery, and recording the capacity, the absolute voltage of the battery, the difference between the auxiliary lug pair and the main lug and the voltage change condition;
step S2: comparing the time when the voltage at different positions reaches a steady state, and drawing a dV/dT curve by taking the time T as an X axis and the dV/dT as a Y axis;
step S3: carrying out differential processing on the dV/dT curve, and drawing by taking the discharge capacity Q as an X axis and the dV/dQ as a Y axis to obtain a dV/dQ curve;
step S4: and judging the rate distribution and the lithium precipitation amount of the lithium ions inserted into the graphite according to the dV/dT curve and the dV/dQ curve.
2. The method for evaluating lithium deposition and uniformity of the large-size soft package lithium ion battery according to claim 1, wherein the step of performing the charge test on the soft package lithium ion battery comprises:
step 101: treating the soft package lithium ion battery at low temperature;
step 102: charging to a specified electric quantity by constant current, and keeping an open circuit;
step 103: and observing and recording the capacity, the absolute voltage of the battery, the difference between the auxiliary pole lug pair and the main pole lug and the voltage change condition.
3. The method for evaluating lithium deposition and uniformity of the large-size soft package lithium ion battery according to claim 2, wherein the step of performing a discharge test on the soft package lithium ion battery comprises:
step 111: treating the soft package lithium ion battery at low temperature;
step 112: discharging immediately after charging to a specified electric quantity with a constant current;
step 113: and observing and recording the capacity, the absolute voltage of the battery, the difference between the auxiliary pole lug pair and the main pole lug and the voltage change condition.
4. The method for evaluating lithium deposition and uniformity of the large-size soft package lithium ion battery according to claim 1 or 3, wherein during discharge, the discharge current is in a range of 0.3-1.0C, and the cut-off voltage is 2.7V.
5. The method for evaluating lithium deposition and uniformity of the large-size soft package lithium ion battery according to claim 3, wherein the temperature value and the current value selected in the charging test step and the discharging test step are consistent.
6. The method for evaluating lithium deposition and uniformity of the large-size soft package lithium ion battery according to claim 3, wherein the low-temperature environment temperature range is from-10 ℃ to 5 ℃.
7. The method for evaluating lithium separation and uniformity of the large-size soft package lithium ion battery according to claim 1, 2 or 3, wherein the tab difference between the auxiliary tab and the main tab is measured by a high-precision analog data recorder.
8. The method for evaluating lithium deposition and uniformity of the large-size soft package lithium ion battery according to claim 1, wherein the step of judging the rate distribution of lithium ion intercalation into graphite and the amount of lithium deposition comprises:
step 401: according to the dV/dT curve, the X axis is time T, the Y axis is dV/dT, any X coordinate is intersected with a corresponding point of the dV/dT curve by taking a perpendicular line as a vertical line, and an intersection point is obtained; making a tangent line of the dV/dT curve through the intersection point, solving the slope of the tangent line, namely the rate of lithium ions embedded into the graphite, and measuring the rate corresponding to the needed X coordinate for multiple times to obtain the rate distribution of the lithium ions embedded into the graphite;
step 402: according to the dV/dQ curve, making a vertical line of any X coordinate and intersecting with a corresponding point of the curve to obtain an intersection point; crossing the crossing point with a horizontal line and crossing the Y axis to obtain a point crossing the Y axis, and calculating the mass of the precipitated lithium according to the formula that m lithium (g) = Q × 3600 × 6.94/96500 by taking the capacity corresponding to the point crossing the Y axis.
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| CN115060320B (en) * | 2022-06-20 | 2023-09-29 | 武汉涛初科技有限公司 | Online monitoring and analyzing system for production quality of power lithium battery based on machine vision |
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