CN114720526A - Rapid evaluation method for cycle performance of lithium iron phosphate material - Google Patents
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Abstract
The invention relates to a rapid evaluation method of the cycle performance of a lithium iron phosphate material, which specifically comprises the following steps: (1) diffusion impedance of a half-cell EIS test of lithium iron phosphate to be tested and a half-cell EIS test of standard lithium iron phosphate respectively; (2) comparing the increase rate of the charge transfer impedance of the EIS test of the negative plate after the battery to be tested and the standard battery are circulated for a certain number of times; (3) judging according to the comparative analysis in the step (1) and the step (2), and if the judgment cannot be made, carrying out the next step; (4) and (5) recording the highest temperature of the center of the surface of the battery in the circulating process of the battery to be tested by testing, and judging again according to the result. The method for rapidly evaluating the cycle performance of the lithium iron phosphate material can rapidly screen and evaluate the lithium iron phosphate material, shortens the evaluation period of the lithium iron phosphate material, and is simple and easy to operate and implement.
Description
Technical Field
The invention belongs to the technical field of lithium ion batteries, and particularly relates to a rapid evaluation method for the cycle performance of a lithium iron phosphate material.
Background
The lithium ion battery has the outstanding advantages of high energy density, no memory effect, long cycle life, quick charge and discharge, less self-discharge and the like, particularly the lithium iron phosphate battery has long and safe cycle life, is widely applied to the energy storage fields of portable equipment, electric automobiles, aerospace and the like, and has great market demand.
The cycle life of the lithium iron phosphate battery can be affected by general materials, manufacturing processes, tests and the like, and the cycle performance of the lithium ion battery can be affected by the quality of the lithium iron phosphate as a core material of the lithium ion battery, so that the evaluation of the lithium iron phosphate as a positive electrode material in a limited time and with high efficiency becomes an important subject of various battery manufacturers.
In the evaluation method of the lithium iron phosphate material in the prior art, the lithium iron phosphate material is generally used as a positive electrode material to prepare a lithium ion battery, and then a normal temperature cycle test is performed, wherein the normal temperature cycle test generally comprises the following steps: the normal temperature 1C charging and discharging requires about 3 hours for 1 cycle test, and the normal temperature cycle test requires 3000 cycles, namely, the time of about 1 year is required to obtain the cycle test result. The lithium iron phosphate is evaluated and screened through a cycle performance test result, but the material test time is long, and the whole test period consumes a long time.
Disclosure of Invention
The invention aims to provide a method for rapidly evaluating the cycle performance of a lithium iron phosphate material, which can rapidly evaluate the cycle performance of the lithium iron phosphate material and is convenient and simple to operate.
The technical scheme adopted by the invention for solving the problems is as follows: a rapid evaluation method for the cycle performance of a lithium iron phosphate material comprises the following steps:
(1) respectively testing electrochemical impedance spectrums EIS of half cells of a standard lithium iron phosphate material L and a lithium iron phosphate material L-1 to be tested to obtain diffusion impedances of the L and the L-1, and respectively recording the diffusion impedances as a diffusion impedance (L) and a diffusion impedance (L-1);
(2) marking a battery made of a standard lithium iron phosphate material L as a standard battery B, marking a battery made of a lithium iron phosphate material L-1 to be tested as a battery B-1 to be tested, carrying out a normal-temperature 1C cycle test on the batteries B and B-1, disassembling the batteries when the batteries are cycled for 100 times and 500 times, taking out a negative plate, assembling a half battery, wherein the negative plates of the batteries B and B-1 are respectively marked as N and N-1, the negative plates of the batteries B and B-1 are respectively marked as N (100) and N-1(100) when the batteries are cycled for 100 times, the negative plates of the batteries B and B-1 are respectively marked as N (500) and N-1(500), and the negative plates of the batteries N (100) and N-1(100), N (500) and N-1(500) are respectively subjected to an electrochemical impedance spectroscopy EIS test to obtain a charge transfer Rct (N (100)), rct (N (500)), Rct (N-1(100)), Rct (N-1 (500));
the battery B-1 to be tested is different from the standard battery B only in that the positive pole lithium iron phosphate material is different, the standard battery B adopts a standard lithium iron phosphate material L with qualified cycle performance, and the positive pole material of the battery B-1 to be tested is the lithium iron phosphate material L-1 to be tested;
(3) carrying out comparative analysis on the result of the step (1), and comparing the magnitude relation of the diffusion impedance (L-1) and the diffusion impedance (L);
(4) calculating the results of the step (2) to obtain the increase rates of the Rct of the standard battery B negative plate and the battery B-1 negative plate to be tested, namely the increase rates of the Rct (N) and the increase rates of the Rct (N-1), and carrying out comparative analysis;
(5) and (4) judging according to the comparative analysis of the step (3) and the step (4):
if the diffusion resistance (L-1) is less than or equal to the diffusion resistance (L) and the growth rate of the Rct (N-1(500)) is less than or equal to the Rct (N (500)), the normal-temperature cycle performance of the lithium iron phosphate material L-1 can be judged to be better than or equal to that of the lithium iron phosphate material L;
if the diffusion resistance (L-1) > the diffusion resistance (L) and the growth rate of the Rct (N-1(500)) is greater than the Rct (N (500)), the normal-temperature cycle performance of the lithium iron phosphate material L-1 can be judged to be worse than that of the lithium iron phosphate material L;
if the diffusion resistance (L-1) ≦ diffusion resistance (L) and the rate of increase of Rct (N-1(500) > Rct (N (500)), proceeding to the next step;
if the diffusion resistance (L-1) > the diffusion resistance (L) and the growth rate of Rct (N-1(500)) is less than or equal to Rct (N (500)), the next step is performed;
(6) in the circulation process, the temperature of the surface centers of a standard battery B and a battery B-1 to be tested is detected and recorded, and the highest temperatures of the surfaces of the standard battery B and the battery B-1 to be tested are respectively marked as T (B) and T (B-1);
(7) and (4) judging again according to the result of the step (6):
diffusion resistance (L-1) is less than or equal to diffusion resistance (L), the growth rate of Rct (N-1(500)) is more than Rct (N (500)), the relationship between T (B-1) and 30 ℃ is further compared, if T (B-1) is less than or equal to 30 ℃, the normal-temperature cycle performance of the lithium iron phosphate material L-1 is judged to be better than or equal to that of the lithium iron phosphate material L, otherwise, if T (B-1) is more than 30 ℃, the normal-temperature cycle performance of the lithium iron phosphate material L-1 is judged to be worse than that of the lithium iron phosphate material L;
diffusion impedance (L-1) > diffusion impedance (L), and the growth rate of Rct (N-1(500)) is less than or equal to Rct (N (500)), further comparing the relation between T (B-1) and 30 ℃ and 35 ℃, if the temperature of 35 ℃ is more than or equal to T (B-1) and more than or equal to 30 ℃, judging that the normal-temperature cycle performance of the lithium iron phosphate material L-1 is better than or equal to that of the lithium iron phosphate material L, and otherwise, if the temperature of T (B-1) is less than or greater than 30 ℃ or more than 35 ℃, judging that the normal-temperature cycle performance of the lithium iron phosphate material L-1 is worse than that of the lithium iron phosphate material L.
Preferably, the normal-temperature cycle test specifically comprises: under the condition of normal temperature, the charging and discharging current of the battery is 1C, the charging and discharging voltage interval is set to be 2.5-3.65V, the battery is kept still both after the charging and the discharging are finished, and the standing time is 30 min.
Preferably, the rate of increase of Rct (N-1) = [ Rct (N-1(500)) -Rct (N-1(100)) ]/Rct (N-1(100)),
rct (N) growth rate = [ Rct (N (500))) -Rct (N (100)) ]/Rct (N (100)).
Compared with the prior art, the invention has the advantages that:
the invention provides a rapid evaluation method for the cycle performance of a lithium iron phosphate material, which can rapidly screen and evaluate the lithium iron phosphate material, shorten the evaluation period of the lithium iron phosphate material, and is simple and easy to operate and implement.
Detailed Description
The present invention will be described in further detail with reference to examples.
Example 1
A rapid evaluation method of a lithium iron phosphate material comprises the following steps:
(1) testing EIS of half cells of a standard lithium iron phosphate material L and a lithium iron phosphate material L-1 to be tested to obtain diffusion impedances of the L and the L-1, and respectively recording the diffusion impedances as the diffusion impedance (L) and the diffusion impedance (L-1);
(2) testing EIS of half batteries of the negative plate of 100 times and 500 times of normal-temperature 1C circulation of a standard battery B and a battery B-1 to be tested to obtain charge transfer internal resistances Rct (N (100)), Rct (N (500)), Rct (N-1(100)), Rct (N-1(500)), and the increase rate of Rct;
(3) the results of step (1) and step (2) are shown in the following table:
TABLE 1 diffusion resistance of different lithium iron phosphate material half-cells
TABLE 2 Charge transfer impedance of negative half-cells of different cells
Note: 125 (47%) represents a retention of 47% for Rct after 500 cycles relative to 100 cycles, and so on.
As can be seen from Table 1, the diffusion impedance (L-1) < the diffusion impedance (L), and from Table 2, the increase of the Rct of the negative electrode N-1 of the battery B-1 to be tested is less than the increase rate of the Rct of the negative electrode N of the standard battery B, so that the normal-temperature cycle performance of the lithium iron phosphate L-1 is judged to be superior to that of the lithium iron phosphate L.
Example 2
A rapid evaluation method of a lithium iron phosphate material comprises the following steps:
(1) testing EIS of half cells of a standard lithium iron phosphate material L and a lithium iron phosphate material L-2 to be tested to obtain diffusion impedance of L and L-2, and respectively recording the diffusion impedance as diffusion impedance (L) and the diffusion impedance (L-2);
(2) testing EIS of half batteries of the negative plate of 100 times and 500 times of normal-temperature 1C circulation of a standard battery B and a battery B-2 to be tested to obtain charge transfer internal resistances Rct (N (100)), Rct (N (500)), Rct (N-2(100)), Rct (N-2(500)) and Rct (N-2(500)), and calculating the growth rate of the Rct;
(3) the results of step (1) and step (2) are shown in the following table:
TABLE 3 diffusion resistance of different lithium iron phosphate material half-cells
TABLE 4 Charge transfer impedance of negative half-cells of different cells
Note: 125 (47%) represents a retention of 47% for Rct after 500 cycles relative to 100 cycles, and so on.
As can be seen from table 3, when the diffusion resistance (L-2) > the diffusion resistance (L), and as can be seen from table 4, the increase in Rct of the negative electrode N-2 of the battery B-2 to be tested is smaller than the increase rate in Rct of the negative electrode N of the standard battery B, it is determined that the normal-temperature cycle performance of the lithium iron phosphate L-2 is inferior to that of the lithium iron phosphate L.
Example 3
A rapid evaluation method of a lithium iron phosphate material comprises the following steps:
(1) testing EIS of half cells of a standard lithium iron phosphate material L and a lithium iron phosphate material L-3 to be tested to obtain diffusion impedances of the L and the L-3, and respectively recording the diffusion impedances as the diffusion impedance (L) and the diffusion impedance (L-3);
(2) testing EIS of half batteries of the negative plate of 100 times and 500 times of normal-temperature 1C circulation of a standard battery B and a battery B-3 to be tested to obtain charge transfer internal resistances Rct (N (100)), Rct (N (500)), Rct (N-3(100)), Rct (N-3(500)), and the increase rate of Rct;
(3) detecting and recording the temperature of the center of the surface of the battery in the circulating process, and recording the highest temperature of the surface of the battery B-3 as T (B-3) =29 ℃;
(4) the results of steps (1) and (2) are shown in the following table:
TABLE 5 diffusion resistance of different lithium iron phosphate material half-cells
TABLE 6 Charge transfer impedance of negative half-cells of different cells
Note: 125 (47%) represents a retention of 47% for Rct after 500 cycles relative to 100 cycles, and so on.
As can be seen from table 5, the diffusion impedance (L-3) < the diffusion impedance (L), and from table 6, it can be seen that the increase of Rct of the negative electrode N-3 of the battery B-3 to be measured is greater than the increase rate of Rct of the negative electrode N of the standard battery B, and T (B-3) =29 ℃ < 30 ℃, then it is determined that the normal-temperature cycle performance of the lithium iron phosphate L-3 is superior to that of the lithium iron phosphate L.
Example 4
A rapid evaluation method of a lithium iron phosphate material comprises the following steps:
(1) testing EIS of half cells of a standard lithium iron phosphate material L and a lithium iron phosphate material L-4 to be tested to obtain diffusion impedances of the L and the L-4, and respectively recording the diffusion impedances as the diffusion impedance (L) and the diffusion impedance (L-4);
(2) testing EIS of the half batteries of the negative plate of the standard battery B and the battery B-4 to be tested, which are circulated for 100 times and 500 times at normal temperature 1C, obtaining electric charge transfer internal resistances Rct (N (100)), Rct (N (500)), Rct (N-4(100)) and Rct (N-4(500)), and calculating the increase rate of Rct;
(3) the temperature of the center of the surface of the battery during the circulation was detected and recorded, and the highest temperature of the surface of the battery B-4 was recorded as T (B-4) =40 ℃.
(4) The results of steps (1) and (2) are shown in the following table:
TABLE 7 diffusion resistance of different lithium iron phosphate material half-cells
TABLE 8 Charge transfer impedance of negative half-cells of different cells
Note: 125 (47%) represents that the retention rate of Rct after 500 cycles to Rct after 100 cycles is 47%, and so on
As can be seen from table 7, the diffusion resistance (L-4) > the diffusion resistance (L), and from table 8, it is seen that the increase in Rct of the negative electrode N-4 of the battery B-4 to be tested is less than the increase rate in Rct of the negative electrode N of the standard battery B, and T (B-4) =40 ℃ > 35 ℃, it is determined that the normal-temperature cycle performance of the lithium iron phosphate L-4 is inferior to that of the lithium iron phosphate L.
In addition to the above embodiments, the present invention also includes other embodiments, and any technical solutions formed by equivalent transformation or equivalent replacement should fall within the scope of the claims of the present invention.
Claims (3)
1. A method for rapidly evaluating the cycle performance of a lithium iron phosphate material is characterized by comprising the following steps: the method comprises the following steps:
(1) respectively testing electrochemical impedance spectrums EIS of half cells of a standard lithium iron phosphate material L and a lithium iron phosphate material L-1 to be tested to obtain diffusion impedances of the L and the L-1, and respectively recording the diffusion impedances as a diffusion impedance (L) and a diffusion impedance (L-1);
(2) marking a battery made of a standard lithium iron phosphate material L as a standard battery B, marking a battery made of a lithium iron phosphate material L-1 to be detected as a battery B-1 to be detected, carrying out a normal-temperature 1C cycle test on the batteries B and B-1, dismantling the batteries after cycling for 100 times and 500 times, taking out a negative plate, assembling a half battery, wherein the negative plates of the batteries B and B-1 are respectively marked as N and N-1, the negative plates of the batteries B and B-1 for 100 times and the batteries of the batteries B and B-1 for 500 times are respectively marked as N (100) and N-1(500), carrying out an electrochemical impedance spectroscopy EIS test on the batteries of N (100) and N-1(100), N (500) and N-1(500) to obtain an internal resistance Rct (N (100)), rct (N (500)), Rct (N-1(100)), Rct (N-1 (500));
the battery B-1 to be tested is different from the standard battery B only in the situation that a positive lithium iron phosphate material is different, the standard battery B adopts a standard lithium iron phosphate material L with qualified cycle performance, and the positive electrode material of the battery B-1 to be tested is the lithium iron phosphate material L-1 to be tested;
(3) carrying out comparative analysis on the result of the step (1), and comparing the magnitude relation of the diffusion impedance (L-1) and the diffusion impedance (L);
(4) calculating the results of the step (2) to obtain the increase rates of the Rct of the standard battery B negative plate and the battery B-1 negative plate to be tested, namely the increase rates of the Rct (N) and the increase rates of the Rct (N-1), and carrying out comparative analysis;
(5) and (4) judging according to the comparative analysis of the step (3) and the step (4):
if the diffusion resistance (L-1) is less than or equal to the diffusion resistance (L) and the growth rate of the Rct (N-1(500)) is less than or equal to the Rct (N (500)), the normal-temperature cycle performance of the lithium iron phosphate material L-1 can be judged to be better than or equal to that of the lithium iron phosphate material L;
if the diffusion resistance (L-1) > the diffusion resistance (L) and the growth rate of the Rct (N-1(500)) is greater than the Rct (N (500)), the normal-temperature cycle performance of the lithium iron phosphate material L-1 can be judged to be worse than that of the lithium iron phosphate material L;
if the diffusion resistance (L-1) is less than or equal to the diffusion resistance (L) and the increase rate of Rct (N-1(500)) is more than Rct (N (500)), the next step is carried out;
if the diffusion resistance (L-1) > the diffusion resistance (L) and the growth rate of Rct (N-1(500)) is less than or equal to Rct (N (500)), the next step is performed;
(6) in the circulation process, the temperature of the surface centers of a standard battery B and a battery B-1 to be tested is detected and recorded, and the highest temperatures of the surfaces of the standard battery B and the battery B-1 to be tested are respectively marked as T (B) and T (B-1);
(7) and (4) judging again according to the result of the step (6):
diffusion resistance (L-1) is less than or equal to diffusion resistance (L), the growth rate of Rct (N-1(500)) is more than Rct (N (500)), the relationship between T (B-1) and 30 ℃ is further compared, if T (B-1) is less than or equal to 30 ℃, the normal-temperature cycle performance of the lithium iron phosphate material L-1 is judged to be better than or equal to that of the lithium iron phosphate material L, otherwise, if T (B-1) is more than 30 ℃, the normal-temperature cycle performance of the lithium iron phosphate material L-1 is judged to be worse than that of the lithium iron phosphate material L;
diffusion impedance (L-1) > diffusion impedance (L), and the growth rate of Rct (N-1(500)) is less than or equal to Rct (N (500)), further comparing the relation between T (B-1) and 30 ℃ and 35 ℃, if the temperature of 35 ℃ is more than or equal to T (B-1) and more than or equal to 30 ℃, judging that the normal-temperature cycle performance of the lithium iron phosphate material L-1 is better than or equal to that of the lithium iron phosphate material L, and otherwise, if the temperature of T (B-1) is less than or greater than 30 ℃ or more than 35 ℃, judging that the normal-temperature cycle performance of the lithium iron phosphate material L-1 is worse than that of the lithium iron phosphate material L.
2. The method for rapidly evaluating the cycle performance of the lithium iron phosphate material according to claim 1, characterized in that: the normal-temperature cycle test specifically comprises the following steps: under the condition of normal temperature, the charging and discharging current of the battery is 1C, the charging and discharging voltage interval is set to be 2.5-3.65V, the battery is kept still both after the charging and the discharging are finished, and the standing time is 30 min.
3. The method for rapidly evaluating cycle performance of a lithium iron phosphate material according to claim 1, wherein an Rct (N-1) growth rate = [ Rct (N-1 (500))) -Rct (N-1(100)) ]/Rct (N-1(100)) ], and an Rct (N) growth rate = [ Rct (N (500)) -Rct (N (100)) ]/Rct (N (100)).
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