CN115032235A - Method for rapidly screening cycle performance of high-voltage lithium cobalt oxide material - Google Patents
Method for rapidly screening cycle performance of high-voltage lithium cobalt oxide material Download PDFInfo
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- 239000000463 material Substances 0.000 title claims abstract description 118
- 238000000034 method Methods 0.000 title claims abstract description 29
- 238000012216 screening Methods 0.000 title claims abstract description 14
- 229910000625 lithium cobalt oxide Inorganic materials 0.000 title abstract description 9
- BFZPBUKRYWOWDV-UHFFFAOYSA-N lithium;oxido(oxo)cobalt Chemical compound [Li+].[O-][Co]=O BFZPBUKRYWOWDV-UHFFFAOYSA-N 0.000 title abstract description 9
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 claims abstract description 65
- 229910052744 lithium Inorganic materials 0.000 claims abstract description 65
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 claims abstract description 21
- 229910001416 lithium ion Inorganic materials 0.000 claims abstract description 21
- 238000007599 discharging Methods 0.000 claims abstract description 13
- 102100027368 Histone H1.3 Human genes 0.000 claims abstract description 10
- 101001009450 Homo sapiens Histone H1.3 Proteins 0.000 claims abstract description 10
- 230000010354 integration Effects 0.000 claims description 13
- 238000012545 processing Methods 0.000 claims description 6
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 4
- 238000010280 constant potential charging Methods 0.000 claims description 4
- 238000010277 constant-current charging Methods 0.000 claims description 4
- 229910002804 graphite Inorganic materials 0.000 claims description 4
- 239000010439 graphite Substances 0.000 claims description 4
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 2
- 239000003792 electrolyte Substances 0.000 claims description 2
- 229910052710 silicon Inorganic materials 0.000 claims description 2
- 239000010703 silicon Substances 0.000 claims description 2
- 238000012360 testing method Methods 0.000 abstract description 9
- 230000002427 irreversible effect Effects 0.000 abstract 1
- 238000010586 diagram Methods 0.000 description 4
- 230000014759 maintenance of location Effects 0.000 description 3
- 238000010998 test method Methods 0.000 description 3
- 229910012820 LiCoO Inorganic materials 0.000 description 2
- 230000001351 cycling effect Effects 0.000 description 2
- 238000005034 decoration Methods 0.000 description 2
- 230000007423 decrease Effects 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000011056 performance test Methods 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000005056 compaction Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 230000002441 reversible effect Effects 0.000 description 1
- 238000007086 side reaction Methods 0.000 description 1
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- G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
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- G—PHYSICS
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
- G01N27/02—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance
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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]
- G01R31/385—Arrangements for measuring battery or accumulator variables
- G01R31/387—Determining ampere-hour charge capacity or SoC
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- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
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- H01M10/425—Structural combination with electronic components, e.g. electronic circuits integrated to the outside of the casing
- H01M2010/4278—Systems for data transfer from batteries, e.g. transfer of battery parameters to a controller, data transferred between battery controller and main controller
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Abstract
The invention belongs to the field of lithium batteries, and particularly relates to a method for rapidly screening the cycle performance of a high-voltage lithium cobalt oxide material, which comprises the following steps: firstly, preparing different lithium ion soft package batteries by adopting different lithium cobaltate materials; secondly, carrying out a charge and discharge test in a preset temperature environment; step three, collecting detailed data of the discharging process in the step two to obtain a dQ/dV-V curve; fourthly, integrating the dQ/dV-V curve to obtain the integral area of the voltage interval, comparing the integral areas of the dQ/dV-V curves of different materials under the voltage interval, and judging the cycle performance of the materials according to the integral areas; the structural stability of the lithium cobaltate material under high voltage is judged according to the existence amount of irreversible H1-3 phase and O1 phase when the high voltage lithium cobaltate material is fully charged, so that the cycle performance of the high voltage lithium cobaltate material is rapidly screened.
Description
Technical Field
The invention belongs to the field of lithium batteries, and particularly relates to a method for rapidly screening the cycle performance of a high-voltage lithium cobalt oxide material.
Background
Lithium cobaltate materials are widely applied in the field of 3C products due to the characteristics of high capacity, high discharge platform and high compaction density. With the gradual increase of the requirements of 3C products on energy density, higher requirements are put forward on the capacity of lithium cobaltate materials, the increase of the use upper limit voltage of lithium cobaltate is an effective way for increasing the capacity of lithium cobaltate, and the use upper limit voltage of commercial lithium cobaltate materials reaches 4.5V at present.
Cycling performance has been a concern as one of the key electrical properties of 3C batteries. The conventional cycle test method has long test period and needs a large amount of test resources, so the method for rapidly screening the cycle performance of the high-voltage lithium cobalt oxide material has important significance and considerable practical use value.
Disclosure of Invention
The invention aims to provide a method for rapidly screening the cycle performance of a high-voltage lithium cobalt oxide material.
In order to achieve the purpose, the invention adopts the technical scheme that:
a method for rapidly screening the cycle performance of a high-voltage lithium cobaltate material is characterized by comprising the following steps:
firstly, preparing different lithium cobaltate materials for the positive electrode, the same negative electrode, a diaphragm and electrolyte according to the same formula and process to obtain different lithium ion batteries;
secondly, under the preset temperature environment, constant current charging is carried out on the series of different lithium ion soft package batteries obtained in the first step by using preset constant current I1 until the lithium ion soft package batteries are charged to a preset voltage U1, then constant voltage charging is carried out by using voltage U1, the cut-off current is I2, then discharging is carried out by using current I3, and discharging is carried out to 3V;
step three, collecting detailed data of the discharging process in the step two, and carrying out differential processing on voltage and capacity data in the data to obtain a dQ/dV-V curve;
and fourthly, performing integration treatment on the dQ/dV-V curve, wherein a voltage interval corresponding to the integration is U1-4.3V, an H1-3 phase and an O1 phase which correspond to the lithium cobaltate material and have irreversibility in the voltage interval are obtained, the integration areas S of the voltage intervals of any two lithium ion batteries are obtained, the area corresponding to the lithium cobaltate material 1 is S1, and the area corresponding to the lithium cobaltate material 2 is S2.
If S1 > S2, the cycle performance of the lithium cobaltate material 1 is inferior to that of the lithium cobaltate material 2.
If S1 < S2, the cycle performance of the lithium cobaltate material 1 is better than that of the lithium cobaltate material 2.
If S1 is equal to S2 and the peak of the dQ/dV-V curve of lithium cobaltate material 1 shifts to the right in the U1-4.3V interval, the electrochemical impedance of lithium cobaltate material 1 is smaller, and the cycle performance of lithium cobaltate material 1 is better than that of lithium cobaltate material 2.
In the first step, the upper limit service voltage of the anode lithium cobaltate material is more than or equal to 4.5V.
In the second step, the preset temperature is 25-45 ℃; the value range of the current I1 is more than 0 and less than 1C, and the value range of the voltage U1 is more than or equal to 4.5V and less than or equal to 4.7V; the value range of the current I2 is more than 0 and less than or equal to 0.05C; the value range of the current I3 is more than 0 and less than or equal to 0.2C.
The negative electrode is selected from a graphite negative electrode or a lithium negative electrode or a silicon-containing negative electrode; the lithium ion battery is one of a soft package battery, a square battery and a button battery.
Compared with the prior art, the invention has the beneficial effects that:
the lithium cobaltate material has the advantages that the crystal structure of the material is changed along with the increase of voltage, and the material is changed from a reversible O3 phase to an H1-3 phase and then to an O1 phase, wherein the H1-3 phase and the O1 phase have irreversibility, the layered structures of the lithium cobaltate material under the H1-3 phase and the O1 phase collapse, side reactions are accelerated, active lithium ions are lost, and the cycle performance of the lithium cobaltate material is deteriorated.
The cycle performance of the conventional lithium cobalt oxide material battery is characterized by the discharge capacity retention rate, the whole cycle test period needs 4-8 months, and the cycle test period is too long, so that the development efficiency of the lithium ion battery is seriously influenced.
According to the method, the number relation of H1-3 phases and O1 phases in different lithium cobaltates is judged by comparing the integral area size of H1-3 phases and O1 corresponding voltage intervals in dQ/dV-V curves in the full-battery discharge process of different lithium cobaltates, the more H1-3 phases and O1 phases exist, the worse the cycle performance of the lithium cobaltate material is, and the high-voltage lithium cobaltate material is rapidly screened according to the principle.
Drawings
FIG. 1 is a schematic diagram of dQ/dV-V obtained by soft package batteries of different types according to the method in example 1, based on the method for rapidly screening the cycle performance of a high-voltage lithium cobalt oxide material provided by the invention;
FIG. 2 is a schematic diagram of the cycle performance test curves of different types of lithium cobaltate soft package batteries in the embodiment 1 at the temperature of 45 ℃;
FIG. 3 is a schematic diagram of dQ/dV-V obtained by different types of lithium cobaltate soft package batteries according to the method in example 2, based on the method for rapidly screening the cycle performance of a high-voltage lithium cobaltate material provided by the invention;
fig. 4 is a schematic diagram of the cycle performance test curve of different types of lithium cobaltate soft package batteries in the embodiment 2 at the temperature of 45 ℃.
Detailed Description
In order to make the technical solutions of the present invention better understood by those skilled in the art, the present invention will be further described in detail with reference to the accompanying drawings and preferred embodiments.
Embodiment 1a method for rapidly screening cycle performance of a high-voltage lithium cobalt oxide material, comprising the following steps:
in the first step, a lithium cobaltate material (LiCoO) is used 2 ) And matching the material A, the material B, the material C and the material D with a graphite cathode to finish the manufacture of series of different 2.2Ah lithium ion soft package batteries.
And secondly, performing constant-current charging on the lithium ion soft package battery at the temperature of 25 ℃ at the preset constant current of 1.1A until the lithium ion soft package battery is charged to the preset voltage of 4.53V, then performing constant-voltage charging at the voltage of 4.53V, stopping the current of 110mA, then discharging at the current of 0.44A, and discharging to the voltage of 3V.
Step three, collecting detailed data of the discharging process in the step two, and carrying out differential processing on voltage and capacity data in the data to obtain a dQ/dV-V curve;
and fourthly, performing integration processing on the dQ/dV-V curve, wherein the voltage interval corresponding to the integration is 4.53-4.3V, and obtaining the integration area of the voltage interval.
Comparing the integral area of the dQ/dV-V curves of the 4 materials in the voltage interval, the larger the integral area is, the worse the cycle performance of the materials is.
FIG. 1 is a dQ/dV-V curve of 4 lithium cobaltate materials in the discharge process, a reduction peak exists at 4.4V, and the dQ/dV-V curve is subjected to integration treatment in an interval of 4.53-4.3V to obtain the integrated areas of the 4 materials in the voltage interval, and the integrated areas are shown in Table 1. The integral area relationship is: the material C < the material B < the material D < the material A, and the existence proportion relation of H1-3 phase and O1 phase of 4 materials under 4.53V is that the material C < the material B < the material D < the material A.
Table 1 shows the integrated areas of the dQ/dV-V curves of different types of lithium cobaltates in the embodiment 1 in the set voltage interval;
TABLE 1
| Material | Integral area |
| Material A | 0.369 |
| Material B | 0.329 |
| Material C | 0.298 |
| Material D | 0.353 |
Fig. 2 is a test curve of 45 ℃ cycle performance of 4 lithium cobaltate material battery systems. The cycle test method was 0.8C charged to 4.53V, cut off with a current of 0.05C, and then 0.5C discharged to 3V, which is one cycle period. And respectively carrying out 0.5C cycle test on the lithium ion soft package batteries of the 4 lithium cobaltate materials A, B, C and D. The better the cycle performance, i.e., the slower the cycle discharge capacity retention rate decreases. As can be seen from fig. 2, the 45 ℃ cycle performance relationship of the 4 materials is: material C > material B > material D > material a, consistent with the regularity results obtained in table 1.
Example 2: a method for rapidly screening the cycle performance of a high-voltage lithium cobaltate material specifically comprises the following steps:
in the first step, a lithium cobaltate material (LiCoO) is used 2 ) And matching the material E, the material F, the material G and the material H with a graphite cathode to finish the manufacture of series of different 2.0Ah lithium ion soft package batteries.
And secondly, performing constant current charging on the lithium ion flexible package battery at the temperature of 25 ℃ by using a preset constant current 1A until the lithium ion flexible package battery is charged to a preset voltage of 4.5V, then performing constant voltage charging at the voltage of 4.5V, stopping the constant current at 50mA, then discharging at the current of 0.2A, and discharging to 3V.
Thirdly, collecting detailed data of the discharging process in the second step, and carrying out differential processing on voltage and capacity data in the data to obtain a dQ/dV-V curve;
and fourthly, performing integration processing on the dQ/dV-V curve, wherein the voltage interval corresponding to the integration is 4.5-4.3V, and obtaining the integration area of the voltage interval.
Comparing the integral area of the dQ/dV-V curves of the 4 materials in the voltage interval, the larger the integral area is, the worse the cycle performance of the materials is.
FIG. 3 is a dQ/dV-V curve of 4 lithium cobaltate materials in the discharge process, a reduction peak exists at 4.4V, and the dQ/dV-V curve is subjected to integration treatment in the interval of 4.5-4.3V to obtain the integrated areas of the 4 materials in the voltage interval, and the integrated areas are shown in Table 2. The integral area relationship is: material F ═ material H < material E < material G, and the dQ/dV-V curve for material F corresponds to a voltage of 4.322V at a peak voltage of 4.5-4.3V, the dQ/dV-V curve for material H corresponds to a voltage of 4.315V at a peak voltage of 4.5-4.3V, the peak voltage for material F is higher than that for material H, the electrochemical impedance of material F is lower than that of material H, and it is presumed that the cycling performance of 4 materials at 4.5V is: material F > material H > material E > material G.
Table 2 shows the integrated areas of the dQ/dV-V curves of the lithium cobaltates of different types in the set voltage interval in embodiment 2;
TABLE 2
Fig. 4 is a test curve of 45 ℃ cycle performance of 4 lithium cobaltate material battery systems. The cycle test method was a 0.8C charge to 4.5V, cut off at a current of 0.05C, and then a 0.5C discharge to 3V, which is one cycle period. And respectively carrying out 0.5C cycle test on the lithium ion soft package batteries of 4 lithium cobaltate materials E, F, G and H. The better the cycle performance, i.e., the slower the cycle discharge capacity retention rate decreases. As can be seen from fig. 2, the 45 ℃ cycle performance relationship of the 4 materials is: the conclusion that the material F is more than the material H is more than the material E is more than the material G is consistent with the conclusion obtained by the patent evaluation method.
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and decorations can be made without departing from the principle of the present invention, and these modifications and decorations should also be regarded as the protection scope of the present invention.
Claims (3)
1. A method for rapidly screening the cycle performance of a high-voltage lithium cobaltate material is characterized by comprising the following steps:
firstly, preparing different lithium cobaltate materials for the positive electrode, the same negative electrode, a diaphragm and electrolyte according to the same formula and process to obtain different lithium ion batteries;
secondly, under the preset temperature environment, constant current charging is carried out on the series of different lithium ion soft package batteries obtained in the first step by using preset constant current I1 until the lithium ion soft package batteries are charged to a preset voltage U1, then constant voltage charging is carried out by using voltage U1, the cut-off current is I2, then discharging is carried out by using current I3, and discharging is carried out to 3V;
step three, collecting detailed data of the discharging process in the step two, and carrying out differential processing on voltage and capacity data in the data to obtain a dQ/dV-V curve;
fourthly, performing integration treatment on the dQ/dV-V curve, wherein a voltage interval corresponding to the integration is U1-4.3V, the H1-3 phase and the O1 phase, which correspond to the lithium cobaltate material, have irreversibility in the voltage interval, so as to obtain the integrated area S of the voltage interval of any two lithium ion batteries, the area corresponding to the lithium cobaltate material 1 is S1, and the area corresponding to the lithium cobaltate material 2 is S2;
if S1 > S2, the cycle performance of the lithium cobaltate material 1 is inferior to that of the lithium cobaltate material 2;
if S1 is less than S2, the cycle performance of the lithium cobaltate material 1 is better than that of the lithium cobaltate material 2;
if S1 is equal to S2 and the peak of the dQ/dV-V curve of lithium cobaltate material 1 shifts to the right in the U1-4.3V interval, the electrochemical impedance of lithium cobaltate material 1 is smaller, and the cycle performance of lithium cobaltate material 1 is better than that of lithium cobaltate material 2.
2. The method for rapidly screening the cycle performance of the high-voltage lithium cobaltate material according to claim 1, wherein the method comprises the following steps:
in the first step, the upper limit service voltage of the anode lithium cobaltate material is more than or equal to 4.5V;
in the second step, the preset temperature is 25-45 ℃; the value range of the current I1 is more than 0 and less than 1C, and the value range of the voltage U1 is more than or equal to 4.5V and less than or equal to 4.7V; the value range of the current I2 is more than 0 and less than or equal to 0.05C; the value range of the current I3 is more than 0 and less than or equal to 0.2C.
3. The method for rapidly screening the cycle performance of the high-voltage lithium cobaltate material according to claim 1, wherein the method comprises the following steps: the negative electrode is selected from a graphite negative electrode or a lithium negative electrode or a silicon-containing negative electrode; the lithium ion battery is one of a soft package battery, a square battery and a button battery.
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