CN112505087A - Thermal stability evaluation method of lithium ion battery electrode material - Google Patents
Thermal stability evaluation method of lithium ion battery electrode material Download PDFInfo
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- CN112505087A CN112505087A CN202011271858.3A CN202011271858A CN112505087A CN 112505087 A CN112505087 A CN 112505087A CN 202011271858 A CN202011271858 A CN 202011271858A CN 112505087 A CN112505087 A CN 112505087A
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N25/00—Investigating or analyzing materials by the use of thermal means
- G01N25/02—Investigating or analyzing materials by the use of thermal means by investigating changes of state or changes of phase; by investigating sintering
- G01N25/12—Investigating or analyzing materials by the use of thermal means by investigating changes of state or changes of phase; by investigating sintering of critical point; of other phase change
Abstract
The invention discloses a method for evaluating the thermal stability of an electrode material of a lithium ion battery, which comprises the following steps: s1, setting a preset temperature T; s2, disassembling the battery cell in the 100% SOC state to obtain an electrode material; s3, obtaining the exothermic temperature T of the reaction of the electrode material and the electrolyte1And the thermal decomposition temperature T of the electrode material2(ii) a S4, mixing T1、T2And comparing the obtained product with T to evaluate whether the thermal stability of the electrode material is qualified or not. The invention provides a simple and reliable method for evaluating the thermal stability of the electrode material, which is beneficial to simply, quickly, accurately and effectively screening the appropriate lithium ion battery electrode material and reducing the thermal runaway risk of the lithium ion battery.
Description
Technical Field
The invention relates to the technical field of battery testing, in particular to a thermal stability evaluation method of a lithium ion battery electrode material.
Background
In all current battery systems, lithium ion batteries can better meet the requirements of vehicles on power output, driving distance, acceleration capacity, service life and energy density. But due to its thermal instability, combustion or explosion may occur under extreme conditions, greatly hindering the practical application of large lithium ion batteries. Namely, among many factors influencing the safety performance of the lithium ion battery, the thermal stability of the electrode material determines the practical use upper and lower limits of the lithium ion battery. Many researches show that the decomposition of the cathode material causes the ignition and explosion of the lithium ion battery, and particularly the cathode material has thermal instability in a higher charging state, so that the risk of thermal runaway exists, the combustion of the electrolyte is further caused, and the ignition and even the explosion of the battery are finally caused. Therefore, in order to meet the safety problem of high-power lithium ion batteries, it is important to evaluate the thermal stability of the electrode material.
Disclosure of Invention
Based on the technical problems in the background art, the invention provides a method for evaluating the thermal stability of an electrode material of a lithium ion battery.
The invention provides a method for evaluating the thermal stability of an electrode material of a lithium ion battery, which comprises the following steps:
s1, setting a preset temperature T;
s2, disassembling the battery cell in the 100% SOC state to obtain an electrode material;
s3, obtaining the exothermic temperature T of the reaction of the electrode material and the electrolyte1And the thermal decomposition temperature T of the electrode material2；
S4, mixing T1、T2Comparing with T if T1、T2If the temperature is greater than T, the thermal stability of the electrode material is qualified; otherwise, the thermal stability of the electrode material is not satisfactory.
Preferably, in step S3, the electrode material is subjected to DSC test to obtain T1And performing TG test to obtain T2。
Preferably, the temperature rise rate of the DSC test is 5-15 ℃/min; preferably, when the electrode material is a positive electrode material, the termination temperature of the DSC test is 200-250 ℃, and when the electrode material is a negative electrode material, the termination temperature of the DSC test is 400-450 ℃.
Preferably, the temperature rise rate of the TG test is 5-15 ℃/min, and the termination temperature is 800-900 ℃.
Preferably, the electrode material is subjected to DSC test and TG test, and then is subjected to powdering treatment after removing the electrolyte.
Preferably, the method for removing the electrolyte comprises the following steps: the electrode material is cleaned by a solvent and then dried.
The powdering treatment needs to be carried out by a method which does not damage the basic structure of the electrode material and does not introduce impurities, and particularly, a grinding method can be adopted.
Preferably, the steps S2 and S3 are performed under oxygen-free conditions.
The invention has the following beneficial effects:
the invention obtains the exothermic temperature T of the reaction of the electrode material and the electrolyte by disassembling the electrode material in the 100% SOC state from the lithium ion battery1And the thermal decomposition temperature T of the electrode material2And comparing the temperature with a preset temperature T so as to evaluate whether the thermal stability of the electrode material is qualified or not. The invention provides a simple and reliable method for evaluating the thermal stability of the electrode material, which is beneficial to simply, quickly, accurately and effectively screening the appropriate lithium ion battery electrode material and reducing the thermal runaway risk of the lithium ion battery.
Drawings
Fig. 1 is a DSC graph of a negative electrode material of example 1.
Fig. 2 is a TG graph of the anode material of example 1.
Fig. 3 is a DSC graph of the positive electrode material of example 2.
Fig. 4 is a TG graph of the cathode material of example 2.
Detailed Description
The technical solution of the present invention will be described in detail below with reference to specific examples.
Example 1
S1, setting the preset temperature T to 260 ℃;
s2, disassembling the LFP battery cell in the 100% SOC state under the inert atmosphere to obtain a negative pole piece, soaking the negative pole piece in DMC for 30min to remove electrolyte, drying, scraping powder, and grinding to obtain negative pole material powder;
s3, under inert atmosphere, loading the negative electrode material powder into an alumina crucible, carrying out TG test at a temperature rise rate of 10k/min, wherein the termination temperature of the test is 800 ℃, and obtaining the exothermic temperature T of the reaction of the negative electrode material and the electrolyte1＝439.68℃；
Under inert atmosphere, loading the negative electrode material powder into a high-pressure crucible, performing DSC test at a temperature rise rate of 10k/min, wherein the termination temperature of the test is 400 ℃, and obtaining the thermal decomposition temperature T of the negative electrode material2＝280.83℃；
S4, mixing T1、T2Comparing with T if T1、T2If the temperature is greater than T, the thermal stability of the battery cathode material is qualified; otherwise, the thermal stability of the battery negative electrode material is unqualified. The results show that: t is1＝439.68℃、T2The thermal stability of the battery negative electrode material is qualified when the temperature is 280.83 ℃ which is higher than T260 ℃.
Example 2
S1, setting the preset temperature T to be 120 ℃;
s2, disassembling an LFP battery cell in a 100% SOC state under an inert atmosphere to obtain a positive pole piece, soaking the positive pole piece in DMC for 30min to remove electrolyte, drying, scraping powder, and grinding to obtain positive material powder;
s3, under inert atmosphere, loading the anode material powder into an alumina crucible, and performing TG test at a temperature rise rate of 10k/min, wherein the termination temperature of the test is 800 ℃, and the exothermic temperature T of the reaction of the anode material and the electrolyte is obtained1＝218.60℃；
Under inert atmosphere, the anode material powder is filled into a high-pressure crucible, DSC test is carried out at the temperature rise rate of 10k/min, the termination temperature of the test is 200 ℃, and the thermal decomposition temperature T of the anode material is obtained2＝125.80℃；
S4, mixing T1、T2Comparing with T if T1、T2If the temperature is higher than T, the thermal stability of the battery anode material is qualified; otherwise, the thermal stability of the battery anode material is unqualified. The results show that: t is1＝218.60℃、T2The temperature of 125.80 ℃ is higher than that of T120 ℃, which shows that the thermal stability of the battery anode material is qualified.
The above description is only for the preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art should be considered to be within the technical scope of the present invention, and the technical solutions and the inventive concepts thereof according to the present invention should be equivalent or changed within the scope of the present invention.
Claims (8)
1. A method for evaluating the thermal stability of an electrode material of a lithium ion battery is characterized by comprising the following steps:
s1, setting a preset temperature T;
s2, disassembling the battery cell in the 100% SOC state to obtain an electrode material;
s3, obtaining the exothermic temperature T of the reaction of the electrode material and the electrolyte1And the thermal decomposition temperature T of the electrode material2；
S4, mixing T1、T2Comparing with T if T1、T2If the temperature is greater than T, the thermal stability of the electrode material is qualified; otherwise, the thermal stability of the electrode material is not satisfactory.
2. The method for evaluating thermal stability of an electrode material for a lithium ion battery according to claim 1, wherein in step S3, the electrode material is subjected to DSC test to obtain T1And performing TG test to obtain T2。
3. The method for evaluating the thermal stability of the electrode material for the lithium ion battery according to claim 2, wherein the temperature rise rate of the DSC test is 5 to 15 ℃/min; preferably, when the electrode material is a positive electrode material, the termination temperature of the DSC test is 200-250 ℃, and when the electrode material is a negative electrode material, the termination temperature of the DSC test is 400-450 ℃.
4. The method for evaluating thermal stability of an electrode material of a lithium ion battery according to claim 2 or 3, wherein the temperature rise rate of the TG test is 5-15 ℃/min, and the termination temperature is 800-900 ℃.
5. The method for evaluating the thermal stability of the electrode material of the lithium ion battery according to any one of claims 2 to 4, wherein the electrode material is subjected to a DSC test and a TG test, and then is subjected to a powdering treatment after removing the electrolyte.
6. The method for evaluating the thermal stability of the electrode material for the lithium ion battery according to claim 5, wherein the method for removing the electrolyte comprises the following steps: the electrode material is cleaned by a solvent and then dried.
7. The method for evaluating thermal stability of an electrode material for a lithium ion battery according to claim 5 or 6, wherein the powdering treatment is grinding.
8. The method for evaluating thermal stability of an electrode material for a lithium ion battery according to any one of claims 1 to 7, wherein each of the steps S2 and S3 is performed under an oxygen-free condition.
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| CN113588708A (en) * | 2021-06-21 | 2021-11-02 | 南方电网电动汽车服务有限公司 | Method for detecting thermal stability of lithium ion battery electrode material |
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Application publication date: 20210316 |