CN110568052A - Method for comparing low-temperature performance of carbon negative electrode material of lithium ion battery - Google Patents
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- 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 discloses a method for comparing low-temperature performance of a carbon cathode material of a lithium ion battery, which comprises the following steps of: (1) preparing an electrode plate from a carbon negative electrode material; (2) assembling the half cell; (3) standing at normal temperature and then circulating; (4) and (5) testing the electrochemical performance after the circulation is finished and the low-temperature standing is finished. According to the method, the test result can be used for quickly and accurately comparing the low-temperature performance of the carbon cathode material, the test process steps are reduced, the test period is shortened, the test cost is effectively saved, and the test efficiency is improved.
Description
Technical Field
The invention relates to a method for testing electrochemical performance of a carbon cathode material, in particular to a method for comparing low-temperature performance of a carbon cathode material of a lithium ion battery.
Background
The lithium ion battery is widely applied to the aspects of energy storage, mobile electronic equipment, electric automobiles and the like, has the advantages of high energy density, no memory effect, small environmental pollution and the like, but the capacity of the lithium ion battery is seriously attenuated along with the reduction of temperature, and the low-temperature performance of the lithium ion battery is improved in order to meet the increasing use requirements of people.
The lithium ion battery comprises a positive electrode, a negative electrode, a diaphragm, electrolyte and the like, wherein most negative electrode materials are graphite carbon materials, and the theoretical specific capacity is 372 mAh/g. With the reduction of the temperature, the available specific capacity of the graphite carbon material is rapidly reduced, lithium can hardly be inserted even at the temperature of minus 20 ℃, and the phenomenon of lithium precipitation is serious, so that the graphite carbon material is the most main reason for rapid attenuation of the battery capacity at low temperature. In winter in northern China, particularly in northeast China, the temperature is usually lower than-20 ℃, and the characteristic of the graphite carbon cathode seriously restricts the use of the lithium ion battery in a low-temperature environment. The method has the advantages that the low-temperature performance of the graphite carbon cathode is rapidly and accurately measured, and the selection of proper graphite carbon as the cathode material of the low-temperature lithium ion battery is of great significance.
at present, most enterprises test the low-temperature performance of graphite carbon cathode materials by assembling the graphite carbon cathode materials and anode materials into a full battery, then placing the full battery in a low-temperature thermostat for charge-discharge cycle test, and judging the quality of the low-temperature performance by comparing the capacity. During high-rate charge and discharge, lithium is easy to be separated from the negative electrode, and lithium dendrites penetrate through the diaphragm to cause potential safety hazards, so that the charge and discharge rate is low and is 0.05C or 0.1C, and the test period is long. Meanwhile, the process of the full battery is complex, the discharge capacity is related to the anode material, and the measurement error is large.
Disclosure of Invention
The invention aims to solve the problems, provides a test method capable of quickly and accurately comparing the low-temperature performance of the carbon cathode material of the lithium ion battery, reduces the process steps, shortens the test period and improves the accuracy.
In order to achieve the purpose, the invention provides a process for comparing the low-temperature performance of a carbon negative electrode material of a lithium ion battery, which comprises the following steps.
(1) Preparing different carbon negative electrode materials by a pulping and slurry coating method to obtain electrode plates, and then assembling the electrode plates and metal lithium plates in a glove box filled with Ar to obtain the half-cell.
(2) and after the half ~ cell is assembled, standing for 6 ~ 8h at normal temperature, circulating for 3 ~ 10 circles under the condition of constant current charge and discharge at 0.1C multiplying power of a LAND CT2001A type cell test system, and discharging to open ~ circuit voltage of 0.1 ~ 0.3V after the next circle is fully charged.
(3) and after the half cell test is stopped, standing for 8 ~ 10 h at normal temperature until the open ~ circuit voltage is stable, and then transferring to a low ~ temperature incubator to stand for 10 ~ 12 h at constant temperature of ~ 10 ℃ to ~ 30 ℃.
(4) the half cell is connected with an electrochemical workstation to test alternating current impedance, the scanning frequency range is 100 KHz ~ 10 mHz, and the amplitude is 5 ~ 10 mV.
(5) and the half cell is connected with an electrochemical workstation, cyclic voltammetry is tested, the scanning range is 0 ~ 1V, the scanning rate is 0.1 ~ 0.3 mV/s, and the number of scanning sections is more than 4.
further, the carbon negative electrode material in the step (1) is graphite, a graphitized carbon material or an amorphous carbon material, and the graphite is natural graphite, artificial graphite or composite graphite.
Further, in the pulping and slurry coating process in the step (1), slurry proportions and coating surface densities of different carbon cathode materials are the same, and the types and the use amounts of electrolytes used for half-cell assembly are the same.
further, in the steps (2) and (3), the standing temperature at normal temperature is 20 ~ 30 ℃.
Further, in the steps (4) and (5), the working electrode of the electrochemical workstation is connected with the positive electrode of the half cell, and the counter electrode and the reference electrode are connected with the negative electrode of the half cell.
The invention has the advantages that the carbon negative electrode material and the metal lithium sheet are assembled into the half cell to independently research the carbon negative electrode material, so that the influence of the positive electrode material can be eliminated, and the low-temperature performance of the carbon negative electrode material can be known in a targeted manner. Meanwhile, the half battery is simpler to assemble than the full battery, the test is convenient, and the cost can be saved and the efficiency can be improved for enterprises. Since the impedance of the carbon negative electrode which is increased sharply at low temperature is the main reason of poor low-temperature performance, the low-temperature performance of the carbon negative electrode material can be compared quickly and accurately and qualitatively by accurately measuring the alternating current impedance at low temperature.
Drawings
FIG. 1 is a process flow diagram of the present invention.
Fig. 2, 4 and 6 are Nyquist plots comparing the ac impedance at low temperatures in the process of the present invention.
FIGS. 3, 5 and 7 are graphs comparing low temperature cyclic voltammograms in the process of the present invention.
Detailed Description
The invention provides a process for comparing the low-temperature performance of a carbon cathode material of a lithium ion battery, which aims to solve the problems of long test period, large error and the like in the prior art.
(1) Preparing different carbon negative electrode materials by a pulping and slurry coating method to obtain electrode plates, and then assembling the electrode plates and metal lithium plates in a glove box filled with Ar to obtain the half-cell.
The method for pulping and coating the pulp comprises the following steps.
a. mixing a carbon negative electrode material, a binder and a conductive agent in a ratio of 91 ~ 93% to 5 ~ 7% to 1 ~ 3% in N ~ methyl pyrrolidone (NMP), controlling the solid content to be 40 ~ 50%, and preparing into slurry, wherein the solid content is preferably 45%.
b. uniformly coating the prepared slurry on a copper foil by using a coating machine, drying in an oven, and controlling the coating surface density to be 6 ~ 8 mg/cm2And cutting the electrode plate into a circular electrode plate with the diameter of 16 mm by using a punching machine. The coating surface density is preferably 6 mg/cm2. The coating surface density is high, the electrolyte is not easy to infiltrate, the battery shelf time is prolonged, and if the shelf time is not enough, the utilization rate of the active substances is low.
the method for assembling the half ~ cell comprises the steps of weighing the prepared electrode plate, baking the electrode plate in a vacuum oven at 80 ~ 100 ℃, transferring the electrode plate into a glove box filled with Ar to assemble the half ~ cell, wherein the negative electrode is a metal lithium plate, and the baking temperature of the vacuum oven is preferably 100 ℃.
(2) and (3) after the half ~ cell is assembled, standing for 6 ~ 8h at normal temperature, using a LAND CT2001A type cell test system to perform constant ~ current charge ~ discharge circulation for 3 ~ 10 circles at the multiplying power of 0.1C, and discharging to the open ~ circuit voltage of 0.1 ~ 0.3V after the next circle is fully charged.
Preferably, the half cell is left to stand at room temperature for 8h after the assembly is completed, cycled at 0.1C rate for 2 cycles using a LAND CT2001A model battery test system, and discharged to an open circuit voltage of 0.2V after the 3 rd cycle is fully charged.
After the half-cell is circulated for two circles, a stable SEI film is formed on the surface of the active material at the moment, the 0.2V open circuit voltage avoids a discharge voltage interval when the SEI film is formed, and meanwhile, the discharge voltage interval does not enter a graphite discharge platform area, so that the graphite has consistent lithium intercalation degree, and the consistency and accuracy of the test are greatly improved.
(3) and after the half cell test is stopped, standing for 8 ~ 10 h at normal temperature until the open ~ circuit voltage is stable, and then transferring to a low ~ temperature incubator to stand for 10 ~ 12 h at constant temperature of ~ 10 ℃ to ~ 30 ℃.
The shelf time is short, the battery cannot be cooled sufficiently, the shelf time is long, the battery can generate self-discharge, and the test accuracy is influenced.
(4) the half cell is connected with an electrochemical workstation to test alternating current impedance, the scanning frequency range is 100 KHz ~ 10 mHz, and the amplitude is 5 ~ 10 mV.
the half cell is connected with an electrochemical workstation, a working electrode is connected with a positive electrode, a counter electrode and a reference electrode are connected with a negative electrode, alternating current impedance is tested, the scanning frequency range is 100 KHz ~ 10 mHz, the amplitude is 5 ~ 10 mV, and the optimal amplitude of 5 mV. is too large, so that the steady state of the cell changes, and the testing accuracy is influenced.
(5) and the half cell is connected with an electrochemical workstation, cyclic voltammetry is tested, the scanning range is 0 ~ 1V, the scanning rate is 0.1 ~ 0.3 mV/s, and the number of scanning sections is more than 4.
the half cell is connected with an electrochemical workstation, a working electrode is connected with a positive electrode, a counter electrode and a reference electrode are connected with a negative electrode, cyclic voltammetry is tested, the scanning range is 0 ~ 1V, the scanning rate is 0.1 ~ 0.3 mV/s, the number of scanning sections is 4, and the scanning rate is preferably 0.2 mV/s.
The following examples are further illustrative and explanatory of the present invention and are not to be construed as limiting the invention in any way.
Example 1
1. Preparing a sample to be tested: 138 g of artificial graphite 1, 2 and 3 samples of the same mass were taken and mixed with conductive agent SP and binder respectivelyPVDF and solvent N-methyl pyrrolidone (NMP) are fully stirred and uniformly mixed according to the mass ratio of 92: 2: 6: 130 to prepare slurry; the prepared slurry was knife-coated on a photolytic copper foil with a thickness of 11 μm by a coater to control the coating surface density to 6 mg/cm2And cutting the dried material into wafer pole pieces with the diameter of 16 mm for later use by a slicing machine, and respectively marking the wafer pole pieces as a pole piece 1, a pole piece 2 and a pole piece 3.
2. Assembling a half cell: and drying and weighing the obtained pole piece, transferring the pole piece into a vacuum oven, processing the pole piece for 10 hours at the temperature of 100 ℃, and transferring the pole piece into a Michelona glove box filled with Ar for half-cell assembly. The assembly sequence is as follows: and (3) sealing the positive electrode shell → the stainless steel gasket → the graphite pole piece → the diaphragm → the metal lithium piece → the stainless steel gasket → the spring plate → the negative electrode shell by using a sealing machine to obtain the assembled half cells which are respectively marked as the half cell 1, the half cell 2 and the half cell 3.
3. the testing comprises the steps of standing the obtained half cell at 25 ℃ for 8 hours, circulating for 2 circles at 0.1C multiplying power by using a LAND CT2001A type cell testing system, discharging to 0.2V of open ~ circuit voltage after the 3 rd circle is fully charged, stopping, standing for 8 hours at 25 ℃ after the stop, then transferring to a low ~ temperature incubator at ~ 20 ℃ for continuously standing for 12 hours, testing the alternating current impedance under the open ~ circuit voltage by using a Shanghai Chenghua electrochemical workstation, setting the frequency range to be 100 KHz ~ 10 mHz, setting the amplitude to be 5 mV, performing cyclic voltammetry after the alternating current impedance is tested, setting the initial voltage to be the open ~ circuit voltage, setting the scanning rate to be 0.2mV/s, setting the number of scanning sections to be 4 sections, scanning in the reverse direction, and drawing two sections of closed curves after the testing, wherein the testing results are respectively shown in a graph 2 and a graph.
Table 1 shows the capacity and capacity retention rate at a discharge rate of 0.1C at normal temperature of 25 ℃ and-20 ℃ after manufacturing a full cell using the artificial graphite 1, the artificial graphite 2, the artificial graphite 3, and the positive electrode lithium cobaltate, respectively.
TABLE 1 results of low-temperature performance test of artificial graphite 1, artificial graphite 2 and artificial graphite 3 full cell
| Item | 0.1C discharge capacity at normal temperature | 0.1C discharge capacity at-20 DEG C | Capacity retention rate |
| Artificial graphite 1 | 2250.0 mAh | 1932.7 mAh | 85.9% |
| Artificial graphite 2 | 2253.1 mAh | 1863.2 mAh | 82.7% |
| Artificial graphite 3 | 2259.3 mAh | 1735.6 mAh | 76.8% |
Referring to fig. 2, fig. 3 and table 1, the experimental results show that: the low-temperature alternating-current impedance and the peak current of the cyclic voltammetry curve of the artificial graphite half-cell are completely consistent with the low-temperature performance change trend of the corresponding full-cell: the higher the low-temperature alternating-current impedance is, the lower the peak current of the cyclic voltammetry curve is, and the lower the low-temperature capacity retention rate is. By adopting the invention, after the half battery is assembled, the same shelf time as that of the full battery is removed, and the low-temperature performance of different carbon cathode materials can be compared only by hours or even tens of minutes, thereby omitting the complicated process steps of the full battery and saving a large amount of test time.
Example 2
1. Preparing a sample to be tested: taking 150 g of natural graphite 1, natural graphite 2 and natural graphite 3 samples with the same mass, respectively and fully stirring and uniformly mixing the samples with a conductive agent SP, a binder PVDF and a solvent N-methyl pyrrolidone (NMP) according to the mass ratio of 92: 2: 6: 130 to prepare slurry; the prepared slurry was knife-coated on a photolytic copper foil with a thickness of 11 μm by a coater to control the coating surface density to 6 mg/cm2And cutting the dried material into wafer pole pieces with the diameter of 16 mm for later use by a slicing machine, and respectively marking the wafer pole pieces as a pole piece 1, a pole piece 2 and a pole piece 3.
2. Assembling a half cell: and drying and weighing the obtained pole piece, transferring the pole piece into a vacuum oven, processing the pole piece for 10 hours at the temperature of 100 ℃, and transferring the pole piece into a Michelona glove box filled with Ar for half-cell assembly. The assembly sequence is as follows: and (3) sealing the positive electrode shell → the stainless steel gasket → the graphite pole piece → the diaphragm → the metal lithium piece → the stainless steel gasket → the spring plate → the negative electrode shell by using a sealing machine to obtain the assembled half cells which are respectively marked as the half cell 1, the half cell 2 and the half cell 3.
3. the testing comprises the steps of standing the obtained half cell at 25 ℃ for 8 hours, circulating for 2 circles at 0.1C multiplying power by using a LAND CT2001A type cell testing system, discharging to 0.2V of open ~ circuit voltage after the 3 rd circle is fully charged, stopping, standing for 8 hours at 25 ℃ after the stop, then transferring to a low ~ temperature incubator at ~ 20 ℃ for continuously standing for 12 hours, testing the alternating current impedance under the open ~ circuit voltage by using a Shanghai Chenghua electrochemical workstation, setting the frequency range to be 100 KHz ~ 10 mHz, setting the amplitude to be 5 mV, performing cyclic voltammetry after the alternating current impedance is tested, setting the initial voltage to be the open ~ circuit voltage, setting the scanning rate to be 0.2mV/s, setting the number of scanning sections to be 4 sections, scanning in the reverse direction, and drawing two sections of closed curves after the testing, wherein the testing results are respectively shown in a graph 4 and a graph.
Table 2 shows the capacity and capacity retention rate at a discharge rate of 0.1C at normal temperature of 25 ℃ and-20 ℃ after the full cell was fabricated using the natural graphite 1, the natural graphite 2, the natural graphite 3, and the positive electrode lithium cobaltate, respectively.
TABLE 2 test results of low-temperature performance of full-cell of natural graphite 1, natural graphite 2 and natural graphite 3
| Item | 0.1C discharge capacity at normal temperature | 0.1C discharge capacity at-20 DEG C | Capacity retention rate |
| Natural graphite 1 | 2247.7 mAh | 1967.3 mAh | 87.5% |
| Natural graphite 2 | 2253.3 mAh | 1908.5 mAh | 84.7% |
| Natural graphite 3 | 2257.5 mAh | 1876.7 mAh | 83.1% |
Referring to fig. 4, fig. 5 and table 2, the experimental results show that: the low-temperature alternating-current impedance and the peak current of the cyclic voltammetry curve of the natural graphite half-cell are completely consistent with the low-temperature performance change trend of the corresponding full-cell: the higher the low-temperature alternating-current impedance is, the lower the peak current of the cyclic voltammetry curve is, and the lower the low-temperature capacity retention rate is. By adopting the invention, after the half battery is assembled, the same shelf time as that of the full battery is removed, and the low-temperature performance of different carbon cathode materials can be compared only by hours or even tens of minutes, thereby omitting the complicated process steps of the full battery and saving a large amount of test time.
Example 3
1. Preparing a sample to be tested: 160 g of composite graphite 1, composite graphite 2 and composite graphite 3 samples with the same mass are respectively and fully stirred and uniformly mixed with a conductive agent SP, a binder PVDF and a solvent N-methyl pyrrolidone (NMP) according to the mass ratio of 92: 2: 6: 130 to prepare slurry; the prepared slurry was knife-coated on a photolytic copper foil with a thickness of 11 μm by a coater to control the coating surface density to 6 mg/cm2And cutting the dried material into wafer pole pieces with the diameter of 16 mm for later use by a slicing machine, and respectively marking the wafer pole pieces as a pole piece 1, a pole piece 2 and a pole piece 3.
2. Assembling a half cell: and drying and weighing the obtained pole piece, transferring the pole piece into a vacuum oven, processing the pole piece for 10 hours at the temperature of 100 ℃, and transferring the pole piece into a Michelona glove box filled with Ar for half-cell assembly. The assembly sequence is as follows: and (3) sealing the positive electrode shell → the stainless steel gasket → the graphite pole piece → the diaphragm → the metal lithium piece → the stainless steel gasket → the spring plate → the negative electrode shell by using a sealing machine to obtain the assembled half cells which are respectively marked as the half cell 1, the half cell 2 and the half cell 3.
3. the testing comprises the steps of standing the obtained half cell at 25 ℃ for 8 hours, circulating for 2 circles at 0.1C multiplying power by using a LAND CT2001A type cell testing system, discharging to 0.2V of open ~ circuit voltage after the 3 rd circle is fully charged, stopping, standing for 8 hours at 25 ℃ after the stop, then transferring to a low ~ temperature incubator at ~ 20 ℃ for continuously standing for 12 hours, testing the alternating current impedance under the open ~ circuit voltage by using a Shanghai Chenghua electrochemical workstation, setting the frequency range to be 100 KHz ~ 10 mHz, setting the amplitude to be 5 mV, performing cyclic voltammetry after the alternating current impedance is tested, setting the initial voltage to be the open ~ circuit voltage, setting the scanning rate to be 0.2mV/s, setting the number of scanning sections to be 4 sections, scanning in the reverse direction, and drawing two sections of closed curves, wherein the testing results are respectively shown in a figure 6 and a figure 7.
Table 3 shows the capacity and capacity retention rate at a discharge rate of 0.1C at normal temperature of 25 ℃ and-20 ℃ after manufacturing the full cell using the composite graphite 1, the composite graphite 2, the composite graphite 3, and the positive electrode lithium cobaltate, respectively.
TABLE 3 test results of low-temperature performance of all-cell composite graphite 1, composite graphite 2 and composite graphite 3
| Item | 0.1C discharge capacity at normal temperature | 0.1C discharge capacity at-20 DEG C | Capacity retention rate |
| Composite graphite 1 | 2257.3 mAh | 1957.6 mAh | 86.7% |
| Composite graphite 2 | 2260.5 mAh | 1883.4 mAh | 83.3% |
| Composite graphite 3 | 2249.8 mAh | 1825.2 mAh | 81.1% |
Referring to fig. 6, fig. 7 and table 3, the experimental results show that: the low-temperature alternating-current impedance and the peak current of the cyclic voltammetry curve of the composite graphite half-cell are completely consistent with the low-temperature performance change trend of the corresponding full-cell: the higher the low-temperature alternating-current impedance is, the lower the peak current of the cyclic voltammetry curve is, and the lower the low-temperature capacity retention rate is. By adopting the invention, after the half battery is assembled, the same shelf time as that of the full battery is removed, and the low-temperature performance of different carbon cathode materials can be compared only by hours or even tens of minutes, thereby omitting the complicated process steps of the full battery and saving a large amount of test time.
although the present invention has been described with reference to the above embodiments, the scope of the present invention is not limited thereto, and modifications, substitutions and the like of the above members are intended to fall within the scope of the present invention without departing from the spirit of the present invention.
Claims (5)
1. A method for comparing the low-temperature performance of a carbon cathode material of a lithium ion battery is characterized by comprising the following steps:
(1) Preparing different carbon cathode materials by a pulping and slurry coating method to obtain electrode plates, and then assembling the electrode plates and metal lithium plates in a glove box filled with Ar to obtain a half-cell;
(2) after the half ~ cell is assembled, the half ~ cell is placed for 6 ~ 8 hours at normal temperature, the constant current charge ~ discharge cycle of the LAND CT2001A type cell test system is 3 ~ 10 circles under the multiplying power of 0.1C, and the discharge is stopped until the open ~ circuit voltage is 0.1 ~ 0.3V after the next circle is fully charged;
(3) after the half ~ cell test is stopped, standing for 8 ~ 10 h at normal temperature until the open ~ circuit voltage is stable, and then transferring to a low ~ temperature incubator to stand for 10 ~ 12 h at constant temperature of ~ 10 ℃ to ~ 30 ℃;
(4) the half cell is connected with an electrochemical workstation to test alternating current impedance, the scanning frequency range is 100 KHz ~ 10 mHz, and the amplitude is 5 ~ 10 mV;
(5) the half cell is connected with an electrochemical workstation, cyclic voltammetry is tested, the scanning range is 0 ~ 1V, the scanning rate is 0.1 ~ 0.3 mV/s, and the number of scanning sections is more than 4.
2. The method according to claim 1, wherein the carbon negative electrode material in the step (1) is graphite, a graphitized carbon material or an amorphous carbon material, and the graphite is natural graphite, artificial graphite or composite graphite.
3. The method of claim 1, wherein in the pulping and slurry coating process in the step (1), slurry proportioning and coating surface density of different carbon negative electrode materials are the same, and the type and the amount of electrolyte used for half-cell assembly are the same.
4. the method according ~ claim 1, wherein the room temperature shelf temperature in steps (2) and (3) is 20 ~ 30 ℃.
5. The method of claim 1, wherein in steps (4) and (5), the electrochemical workstation working electrode is connected to the half-cell positive electrode, and the counter electrode and the reference electrode are connected to the half-cell negative electrode.
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Application publication date: 20191213 |