CN111122627A - Method for testing optimal compaction density of graphite negative plate - Google Patents
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 86
- 229910002804 graphite Inorganic materials 0.000 title claims abstract description 82
- 239000010439 graphite Substances 0.000 title claims abstract description 82
- 238000005056 compaction Methods 0.000 title claims abstract description 58
- 238000012360 testing method Methods 0.000 title claims abstract description 52
- 238000000034 method Methods 0.000 title claims abstract description 22
- 238000004519 manufacturing process Methods 0.000 claims abstract description 9
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 claims abstract description 7
- 229910052744 lithium Inorganic materials 0.000 claims abstract description 7
- 238000010998 test method Methods 0.000 claims description 11
- 238000003825 pressing Methods 0.000 claims description 8
- 238000005520 cutting process Methods 0.000 claims description 4
- 229910001416 lithium ion Inorganic materials 0.000 abstract description 5
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 abstract description 4
- 239000013078 crystal Substances 0.000 description 6
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 4
- 238000005096 rolling process Methods 0.000 description 4
- 230000000052 comparative effect Effects 0.000 description 3
- 230000009286 beneficial effect Effects 0.000 description 2
- 229910052802 copper Inorganic materials 0.000 description 2
- 239000010949 copper Substances 0.000 description 2
- 238000009792 diffusion process Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 235000012431 wafers Nutrition 0.000 description 2
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 239000013543 active substance Substances 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 238000012790 confirmation Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000009831 deintercalation Methods 0.000 description 1
- 239000003792 electrolyte Substances 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 238000005087 graphitization Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 238000004804 winding Methods 0.000 description 1
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N23/00—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00
- G01N23/20—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by using diffraction of the radiation by the materials, e.g. for investigating crystal structure; by using scattering of the radiation by the materials, e.g. for investigating non-crystalline materials; by using reflection of the radiation by the materials
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N23/00—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00
- G01N23/20—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by using diffraction of the radiation by the materials, e.g. for investigating crystal structure; by using scattering of the radiation by the materials, e.g. for investigating non-crystalline materials; by using reflection of the radiation by the materials
- G01N23/20008—Constructional details of analysers, e.g. characterised by X-ray source, detector or optical system; Accessories therefor; Preparing specimens therefor
- G01N23/2005—Preparation of powder samples therefor
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N23/00—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00
- G01N23/20—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by using diffraction of the radiation by the materials, e.g. for investigating crystal structure; by using scattering of the radiation by the materials, e.g. for investigating non-crystalline materials; by using reflection of the radiation by the materials
- G01N23/2055—Analysing diffraction patterns
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N2223/00—Investigating materials by wave or particle radiation
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- G01N2223/00—Investigating materials by wave or particle radiation
- G01N2223/05—Investigating materials by wave or particle radiation by diffraction, scatter or reflection
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- G01N2223/0566—Investigating materials by wave or particle radiation by diffraction, scatter or reflection diffraction analysing diffraction pattern
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
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- G01N2223/60—Specific applications or type of materials
- G01N2223/633—Specific applications or type of materials thickness, density, surface weight (unit area)
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Abstract
The invention belongs to the technical field of lithium ion batteries, and particularly relates to a method for testing the optimal compaction density of a graphite negative plate, which comprises the following steps: s1, manufacturing N target graphite pole pieces with different compaction densities and the same area; s2, respectively carrying out XRD test on the N target graphite pole pieces, and calculating the diffraction peak intensity ratio of the N target graphite pole pieces, wherein the diffraction peak intensity ratio is the ratio of I (002) to I (004); s3, respectively taking N target graphite pole pieces as positive electrodes and lithium pieces as negative electrodes to obtain N target button cells; s4, performing charge and discharge tests on the N target button cells respectively, and testing gram capacities of the N target button cells; and S5, taking the diffraction peak intensity ratio of the target graphite pole piece in the target button cell with the maximum gram capacity as the optimal diffraction peak intensity ratio, and taking the compaction density corresponding to the optimal diffraction peak intensity ratio as the optimal compaction density. Compared with the prior art, the method can measure the optimal compaction density more simply and accurately.
Description
Technical Field
The invention belongs to the technical field of lithium ion batteries, and particularly relates to a method for testing the optimal compaction density of a graphite negative plate.
Background
Lithium ion batteries have attracted extensive attention because of their advantages of high safety, long cycle life, environmental friendliness, and relatively low price, and have been widely used in the fields of mobile phones, electric vehicles, and other electric devices.
The lithium ion battery mainly comprises a pole piece, a diaphragm and electrolyte. The compaction density of the pole piece belongs to a very important parameter in the production and preparation of the pole piece, different main materials and corresponding formulas have different optimal compaction densities, and the compaction density has influences on various aspects such as the cycle performance, the multiplying power and a lithium precipitation window of the battery. If the compaction density is too high, the impedance born by the lithium deintercalation in the charge and discharge process of the battery cell is increased, so that the charge and discharge capacity of the battery cell is reduced, and the cycle performance of the battery cell is deteriorated; if the compaction density is too low, the space occupied by the winding production of the battery core becomes larger, so that the quality of the active substance of the whole battery core is reduced, and the whole capacity is reduced. Therefore, an optimal compaction density is closely related to the performance of the battery cell, and the performance of the battery cell is determined, so that it is very critical how to accurately judge the optimal compaction density of a system.
In the analysis of XRD diffraction pattern of negative graphite pole piece, OI value is an important parameter, and according to the related literature report, the graphite orientation is to Li+Diffusion is of greater influence, with smaller I (004) peaks and larger I (110) peaks, i.e., smaller OI values, favoring diffusion, but in reality it is well controlled. Chinese patent 201810372835.8 discloses a method for determining the optimum compaction density by using OI value, but in the actual process, the variation of the OI value is often different and not differentThe difference of the OI values of the pole pieces with the same compaction density is almost the same, the data of different test times of the OI value test of the same pole piece are also greatly different, and the OI value data of the negative pole pieces with different rolling pressures are also overlapped, as shown in figure 2. In addition, in the actual XRD test, the graphite (110) plane peak is often masked by the copper (220) plane peak (as shown in fig. 1), so the accuracy of peak searching is affected, and the obtained peak intensities are different, which is also the main reason for the different sizes of the OI values.
Disclosure of Invention
The invention aims to: aiming at the defects of the prior art, the method for testing the optimal compaction density of the graphite negative plate is provided, and the optimal compaction density of the graphite negative plate can be tested more simply and accurately.
In order to achieve the purpose, the invention adopts the following technical scheme:
a test method for the optimal compaction density of a graphite negative plate comprises the following steps:
s1, manufacturing N target graphite pole pieces with different compaction densities and the same area;
s2, respectively carrying out XRD test on the N target graphite pole pieces, and calculating the diffraction peak intensity ratio of the N target graphite pole pieces, wherein the diffraction peak intensity ratio is the ratio of I (002) to I (004);
s3, respectively taking the N target graphite pole pieces as positive electrodes and the lithium piece as negative electrodes to obtain N target button cells;
s4, performing charge and discharge tests on the N target button cells respectively, and testing gram capacities of the N target button cells;
and S5, taking the diffraction peak intensity ratio of the target graphite pole piece in the target button cell with the maximum gram capacity as the optimal diffraction peak intensity ratio, wherein the compaction density corresponding to the optimal diffraction peak intensity ratio is the optimal compaction density.
As an improvement of the method for testing the optimal compaction density of the graphite negative electrode sheet, step S1 specifically includes:
s11, cutting the graphite pole pieces with the same surface density into N graphite pole pieces with preset areas;
and S12, cold pressing the N graphite pole pieces at different pressures to obtain the target graphite pole pieces with different compaction densities and the same areas.
As an improvement of the test method for the optimal compaction density of the graphite negative plate, an increasing relation is presented among N different pressure values.
As an improvement of the method for testing the optimal compacted density of the graphite negative electrode sheet, in step S3, the target graphite negative electrode sheet is baked before being made into a target button cell.
As an improvement of the test method for the optimal compacted density of the graphite negative electrode sheet, the target graphite negative electrode sheet is baked at 100-120 ℃, and the baking time is at least 4 hours.
As an improvement of the test method for the optimal compaction density of the graphite negative electrode sheet, the model of the target button cell is any one of CR2430, CR2016, CR2032, CR2025, CR1632 and CR 1620.
As an improvement of the method for testing the optimum compacted density of the graphite negative electrode sheet according to the present invention, in step S4, a charge-discharge test was performed at a constant current of 0.05C.
As an improvement of the method for testing the optimal compaction density of the graphite negative electrode sheet, in step S4, the charge cut-off voltage of the charge and discharge test is 2.0V.
As an improvement of the method for testing the optimal compaction density of the graphite negative electrode sheet, in step S4, the discharge cut-off voltage of the charge and discharge test is 0.01V.
Compared with the prior art, the invention at least has the following beneficial effects:
1) the (002) crystal surface peak and the (004) crystal surface peak are important parameters for calculating the graphitization degree, and the ratio of I (002)/I (004) is selected as a judgment basis to be traceable, so that the measured optimal compaction density value is more reliable.
2) According to the invention, XRD test is carried out on the pole pieces with different rolling pressures by taking the peak intensity ratio data of I (002) and I (004) as the basis, on one hand, the data of I (002)/I (004) test is more stable than the OI value, on the other hand, the peak searching difficulty is avoided for the (002) crystal face peak and the (004) crystal face peak, and the XRD map can be found quickly and accurately, so that the data of I (002)/I (004) test is easier to obtain and accurate than the OI value, and the measured optimal compaction density is more accurate.
3) The method can accurately and reliably measure the optimal compaction density, further reduce repeated tests in actual production, facilitate the confirmation of the optimal process, save resources and time and improve production benefits.
4) The method can accurately and reliably measure the optimal compaction density, is favorable for improving the charge-discharge cycle performance, the rate cycle performance and other performances of the battery, and prolongs the service life of the battery.
Drawings
Fig. 1 is an XRD test pattern of the graphite pole piece.
FIG. 2 is a graph showing OI values of the pole pieces measured in step S2 in the comparative example.
FIG. 3 is a graph comparing OI values and I (002)/I (004) in XRD analysis at 40T cold pressing pressure.
FIG. 4 is a graph of gram capacity of graphite pole pieces of varying compaction densities.
Detailed Description
The present invention will be described in further detail with reference to the following detailed description and the accompanying drawings, but the embodiments of the invention are not limited thereto.
Examples
A test method for the optimal compaction density of a graphite negative plate comprises the following steps:
s1, cutting the graphite pole pieces with the same surface density into N graphite pole pieces with preset areas (small wafers with the diameter of 14 mm), and performing cold pressing on the N graphite pole pieces with different pressures (20T, 30T, 40T, 50T, 60T and 70T) respectively to obtain N target graphite pole pieces with different compaction densities and the same areas;
s2, respectively carrying out XRD test on the N target graphite pole pieces, and calculating the diffraction peak intensity ratio of the N graphite pole pieces, wherein the diffraction peak intensity ratio is the ratio of I (002) to I (004);
s3, baking the N target graphite pole pieces at 100-120 ℃ for at least 4h, and then respectively taking the N target graphite pole pieces as positive electrodes and the lithium pieces as negative electrodes to obtain N target button batteries (the model is CR 2430);
s4, performing charge and discharge tests on the N target button cells at a constant current of 0.05C, wherein the charge cut-off voltage is 2.0V, the discharge cut-off voltage is 0.01V, and the gram capacity of the N target button cells is tested;
and S5, taking the diffraction peak intensity ratio of the target graphite pole piece in the target button cell with the maximum gram capacity as the optimal diffraction peak intensity ratio, and taking the compaction density corresponding to the optimal diffraction peak intensity ratio as the optimal compaction density.
Comparative example
A test method for the optimal compaction density of a graphite negative plate comprises the following steps:
s1, cutting the graphite pole pieces with the same surface density into N graphite pole pieces with preset areas (small wafers with the diameter of 14 mm), and performing cold pressing on the N graphite pole pieces with different pressures (20T, 30T, 40T, 50T, 60T and 70T) respectively to obtain N target graphite pole pieces with different compaction densities and the same areas;
s2, respectively carrying out XRD test on the N target graphite pole pieces, and calculating OI values of the N target graphite pole pieces, wherein the OI value is the ratio of I (004) to I (110);
s3, baking the N target graphite pole pieces at 100-120 ℃ for at least 4h, and then respectively taking the N target graphite pole pieces as positive electrodes and the lithium pieces as negative electrodes to obtain N target button batteries (the model is CR 2430);
s4, performing charge and discharge tests on the N target button cells at a constant current of 0.05C, wherein the charge cut-off voltage is 2.0V, the discharge cut-off voltage is 0.01V, and the gram capacity of the N target button cells is tested;
and S5, taking the OI value of the target graphite pole piece in the target button cell with the maximum gram capacity as the optimal OI value, and taking the compaction density corresponding to the optimal OI value as the optimal compaction density.
Performance testing
1) Step S2 of the comparative example was repeated a plurality of times, and the OI values obtained from the plurality of tests were plotted, as shown in fig. 1.
2) And (3) taking the target graphite pole piece obtained when the cold pressing pressure is 40T, repeating the step S2 for multiple times, and testing the diffraction peak intensity ratio (I (002): i (004)) and OI value (I (004): i (110)) were plotted, and the results are shown in table 1 and fig. 2.
3) And calculating the compaction density of the target graphite pole piece obtained after cold pressing at different pressures in implementation, and making a curve graph of the measured gram capacity and the corresponding compaction density, wherein the specific results are shown in table 2 and fig. 3.
Test results
TABLE 1 diffraction Peak intensity ratio and OI value
TABLE 2 compacted Density and gram Capacity
| | |
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50T | 60T | 70T | ||
| Compacted density (g/cm)3) | 1.35 | 1.41 | 1.45 | 1.51 | 1.47 | 1.49 | ||
| Gram capacity (mAh/g) | 351.21 | 353.64 | 356.79 | 355.11 | 354.53 | 353.87 |
As can be seen from FIG. 1, in the actual XRD test, the graphite (110) plane peak is often masked by the copper (220) plane peak, so that the accuracy of peak searching is affected, and the obtained peak intensities are different, which is also the main reason for the difference of the OI values. And for the (002) crystal plane peak and the (004) crystal plane peak, the related peak searching difficulty is avoided, and the XRD spectrum can be found quickly and accurately, so that the data of the I (002)/I (004) test is more stable and reliable than the OI value.
As can be seen from FIG. 2, the data obtained by the OI value of the same graphite electrode piece in multiple tests have large difference, and the OI value data of the graphite electrode piece are overlapped under different cold pressing pressures, that is, the OI value is poor in accuracy. In addition, as can be seen from table 1 and fig. 3, the present invention uses the peak intensity ratio data of I (002) and I (004) as the basis to perform XRD test on the pole pieces with different rolling pressures, and compares the data of I (002)/I (004) and OI values at 40T pressure, which shows that the data of I (002)/I (004) test is more stable than that of OI value.
In summary, the data from the I (002)/I (004) test is more readily available and accurate than the OI values, and the optimum compaction density is more accurately determined. Furthermore, the accurate and reliable optimal compaction density can reduce repeated tests in actual production, is convenient for confirming an optimal process, saves resources and time, improves production benefits, is beneficial to improving the charge-discharge cycle performance, the multiplying power cycle performance and the like of the battery, and prolongs the service life of the battery.
Variations and modifications to the above-described embodiments may also occur to those skilled in the art, which fall within the scope of the invention as disclosed and taught herein. Therefore, the present invention is not limited to the above-mentioned embodiments, and any obvious improvement, replacement or modification made by those skilled in the art based on the present invention is within the protection scope of the present invention. Furthermore, although specific terms are employed herein, they are used in a generic and descriptive sense only and not for purposes of limitation.
Claims (9)
1. The test method for the optimal compaction density of the graphite negative plate is characterized by comprising the following steps:
s1, manufacturing N target graphite pole pieces with different compaction densities and the same area;
s2, respectively carrying out XRD test on the N target graphite pole pieces, and calculating the diffraction peak intensity ratio of the N target graphite pole pieces, wherein the diffraction peak intensity ratio is the ratio of I (002) to I (004);
s3, respectively taking the N target graphite pole pieces as positive electrodes and the lithium piece as negative electrodes to obtain N target button cells;
s4, performing charge and discharge tests on the N target button cells respectively, and testing gram capacities of the N target button cells;
and S5, taking the diffraction peak intensity ratio of the target graphite pole piece in the target button cell with the maximum gram capacity as the optimal diffraction peak intensity ratio, wherein the compaction density corresponding to the optimal diffraction peak intensity ratio is the optimal compaction density.
2. The method for testing the optimal compaction density of the graphite negative electrode sheet according to claim 1, wherein the step S1 specifically comprises the following steps:
s11, cutting the graphite pole pieces with the same surface density into N graphite pole pieces with preset areas;
and S12, cold pressing the N graphite pole pieces at different pressures to obtain the target graphite pole pieces with different compaction densities and the same areas.
3. The test method for the optimal compaction density of the graphite negative electrode sheet according to claim 2, wherein N different pressure values represent an increasing relationship.
4. The test method for the optimal compaction density of the graphite negative electrode sheet according to claim 1, is characterized in that: in step S3, before the target graphite electrode sheet is manufactured into the target button cell, the target graphite electrode sheet is baked.
5. The test method for the optimal compaction density of the graphite negative electrode sheet according to claim 4, is characterized in that: and baking the target graphite pole piece at 100-120 ℃ for at least 4 h.
6. The test method for the optimal compaction density of the negative graphite electrode sheet according to claim 1, wherein the model of the target button cell is any one of CR2430, CR2016, CR2032, CR2025, CR1632 and CR 1620.
7. The method for testing the optimum compacted density of the graphite negative electrode sheet according to claim 1, wherein in step S4, a charge-discharge test is performed at a constant current of 0.05C.
8. The method for testing the optimal compaction density of the graphite negative electrode sheet according to claim 1, wherein in step S4, the charge cut-off voltage of the charge and discharge test is 2.0V.
9. The method for testing the optimal compaction density of the graphite negative electrode sheet according to claim 1, wherein in step S4, the discharge cut-off voltage of the charge and discharge test is 0.01V.
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| CN114975879A (en) * | 2022-05-26 | 2022-08-30 | 湖南立方新能源科技有限责任公司 | Method for determining compacted density of lithium ion battery pole piece |
| CN117664790A (en) * | 2024-02-02 | 2024-03-08 | 深圳三思纵横科技股份有限公司 | Intelligent control method and system of battery powder compaction density test machine |
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| CN113777491B (en) * | 2021-08-27 | 2024-05-03 | 合肥国轩高科动力能源有限公司 | Gram capacity detection method for negative electrode material of invalid lithium ion battery |
| CN114975879A (en) * | 2022-05-26 | 2022-08-30 | 湖南立方新能源科技有限责任公司 | Method for determining compacted density of lithium ion battery pole piece |
| CN117664790A (en) * | 2024-02-02 | 2024-03-08 | 深圳三思纵横科技股份有限公司 | Intelligent control method and system of battery powder compaction density test machine |
| CN117664790B (en) * | 2024-02-02 | 2024-04-05 | 深圳三思纵横科技股份有限公司 | Intelligent control method and system of battery powder compaction density test machine |
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