CN110926966A - Method for detecting safety of lithium ion battery diaphragm - Google Patents
Method for detecting safety of lithium ion battery diaphragm Download PDFInfo
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- CN110926966A CN110926966A CN201911284857.XA CN201911284857A CN110926966A CN 110926966 A CN110926966 A CN 110926966A CN 201911284857 A CN201911284857 A CN 201911284857A CN 110926966 A CN110926966 A CN 110926966A
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N3/00—Investigating strength properties of solid materials by application of mechanical stress
- G01N3/30—Investigating strength properties of solid materials by application of mechanical stress by applying a single impulsive force, e.g. by falling weight
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N2203/00—Investigating strength properties of solid materials by application of mechanical stress
- G01N2203/0058—Kind of property studied
- G01N2203/006—Crack, flaws, fracture or rupture
- G01N2203/0067—Fracture or rupture
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N2203/00—Investigating strength properties of solid materials by application of mechanical stress
- G01N2203/0058—Kind of property studied
- G01N2203/0069—Fatigue, creep, strain-stress relations or elastic constants
- G01N2203/0075—Strain-stress relations or elastic constants
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N2203/00—Investigating strength properties of solid materials by application of mechanical stress
- G01N2203/02—Details not specific for a particular testing method
- G01N2203/022—Environment of the test
- G01N2203/0222—Temperature
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N2203/00—Investigating strength properties of solid materials by application of mechanical stress
- G01N2203/02—Details not specific for a particular testing method
- G01N2203/026—Specifications of the specimen
- G01N2203/0262—Shape of the specimen
- G01N2203/0278—Thin specimens
- G01N2203/0282—Two dimensional, e.g. tapes, webs, sheets, strips, disks or membranes
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N2203/00—Investigating strength properties of solid materials by application of mechanical stress
- G01N2203/02—Details not specific for a particular testing method
- G01N2203/06—Indicating or recording means; Sensing means
- G01N2203/067—Parameter measured for estimating the property
- G01N2203/0676—Force, weight, load, energy, speed or acceleration
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N2203/00—Investigating strength properties of solid materials by application of mechanical stress
- G01N2203/02—Details not specific for a particular testing method
- G01N2203/06—Indicating or recording means; Sensing means
- G01N2203/067—Parameter measured for estimating the property
- G01N2203/0682—Spatial dimension, e.g. length, area, angle
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N2203/00—Investigating strength properties of solid materials by application of mechanical stress
- G01N2203/02—Details not specific for a particular testing method
- G01N2203/06—Indicating or recording means; Sensing means
- G01N2203/067—Parameter measured for estimating the property
- G01N2203/0694—Temperature
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Abstract
The invention relates to the field of high polymer material detection, in particular to a method for detecting the safety of a lithium ion battery diaphragm; the detection method comprises the steps that a steel needle penetrates through a diaphragm, wherein the speed of the steel needle penetrating through the diaphragm is 0.01-100 mm/s; wherein, the steel needle is internally provided with a thermal resistance wire and a temperature probe, and the conical angle of the needle point of the steel needle is 45-60 degrees. The detection method can reflect the deformation process of the diaphragm along with the steel needle in the initial needling process, and can also reflect the hot melting process of the diaphragm under the condition of lower ohmic heat; the method has higher conformity with the actual conditions of the lithium ion battery, and can more accurately reflect the safety performance of the battery under the conditions of internal short circuit, needling and the like compared with the conventional test methods (such as DSC, thermal shrinkage and the like), thereby providing more reliable evidence for the design and material selection of the safety battery.
Description
Technical Field
The invention relates to the field of high polymer material detection, in particular to a method for detecting the safety of a lithium ion battery diaphragm.
Background
With the popularization and application of lithium ion batteries in daily life, the safety problem of the lithium ion batteries is concerned more and more widely. The diaphragm is used as an important component of the lithium ion battery and plays a role in separating a positive electrode from a negative electrode in the battery; if the positive and negative electrodes of the battery are short-circuited due to the breakage of the separator caused by process defects (dust, burrs, lithium dendrites, etc.), external force extrusion, needling, etc., the battery may be subjected to dangerous situations such as fire, explosion, etc.; therefore, as a first valve for battery safety, the safety performance of the separator is very important to the safety performance of the battery as a whole.
The needle prick test is an important test for evaluating the safety behavior of the battery short circuit. In the needling process, the steel needle extrudes the battery core to cause local deformation and cause local short circuit; the degree of local short circuit and the propagation speed of the short-circuited area are closely related to the strength and thermal stability of the separator, and determine whether the battery is thermally runaway, ignited, etc. At present, in the conventional test of the diaphragm, the strength is mainly measured by a puncture tensile machine; the thermal stability is mainly evaluated by DSC, thermal shrinkage rate under baking at different temperatures, film breaking temperature of the diaphragm and the like; these steady-state testing methods do not accurately reflect the safety performance of the cell under the dual force-heat stress of the separator during the needling process. In the needling process, the steel needle extrudes the battery core to cause local short circuit, releases heat, and causes the diaphragm to melt, shrink and the like. The damage degree of the diaphragm caused by external force determines the heat generation of the initial short circuit, and the initial heat generation amount and the thermal stability of the diaphragm determine the initial expansion speed of the short circuit area; with the enlargement of the short circuit area, the ohmic heat generated by the short circuit rises sharply and induces other heat-generating side reactions in the battery; the mutual coupling of various heat and diaphragm short circuit areas finally leads to the fact that the battery enters an uncontrollable self-heating stage, and the battery is out of control thermally. Therefore, in the initial stage of needling, the short circuit degree of the battery is reduced, the large-area short circuit of the battery is avoided, and the needling safety of the battery is an important means. Therefore, the deformation of the diaphragm under the external force, the rupture condition and the expansion condition of the broken hole area of the diaphragm under different temperatures are very important for the safety of the battery needling process.
CN105445313A discloses a method for detecting the thermal stability of a battery diaphragm, which adopts a soldering iron with the temperature of more than 200 ℃ to pierce the diaphragm paved on a metal conductor plate/a glass plate and stands for more than 1s, and measures the thermal stability of the diaphragm by measuring the diameter of the pierced hole of the diaphragm; compared with the traditional baking method, the method has certain advantages, and can more accurately reflect the thermal expansion stability of the diaphragm during local overheating; however, the method is a static test method, can only reflect the change condition of the broken hole area of the diaphragm at local high temperature, has a certain difference from the actual condition, and cannot reflect the deformation process of the diaphragm along with a steel needle in the initial needling process and the hot melting process of the diaphragm under the condition of smaller ohmic heat.
CN104048987A discloses a lithium ion battery diaphragm heat puncturing device and a testing method thereof, the application of the patent aims at simulating the heat puncturing capability of a diaphragm at different temperatures, a testing operation platform is placed in a transparent oven environment, a heating device is connected to a puncturing needle, and the puncturing capability of the diaphragm at high temperature is quantitatively compared by recording the transverse and longitudinal widths of a puncturing opening; the device is provided with mutually vertical graduated scales at the intersection point of the puncture hole, and the transverse width and the longitudinal width of the puncture hole can be quantitatively compared through the graduated scales after the diffusion of the puncture hole of the diaphragm is stable; but from a test method perspective, the method characterizes the heat expansion area of the membrane at local overheating at high temperature, and from a substantial perspective, the thermal stability of the membrane at high temperature is also quantified.
CN109187172A discloses a device and a test method for detecting puncture strength of a membrane, wherein the device and the test method control the temperature, humidity, puncture speed and displacement of the environment, limit the size of the membrane, measure the thickness of the membrane, control a puncture needle to puncture the membrane through a driving mechanism, record puncture force by a sensor, take the average value of three times of measurement, and calculate puncture strength; the method has complete and strict process, but can only reflect the puncture strength of the diaphragm at a specific puncture speed, and has larger difference with the change condition of the diaphragm under the double stress of force and heat in the actual short circuit process of the battery.
In view of the above, the present invention is particularly proposed.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provides a method for detecting the safety of a lithium ion battery diaphragm; the method is particularly suitable for detecting the safety performance of the lithium ion battery diaphragm under external force or high temperature.
Specifically, the detection method comprises the steps that a steel needle penetrates through a septum, and the speed of the steel needle penetrating through the septum is 0.01-100 mm/s;
wherein, the steel needle is internally provided with a thermal resistance wire and a temperature probe, and the conical angle of the needle point of the steel needle is 45-60 degrees.
The detection method can reflect the deformation process of the diaphragm along with the steel needle in the initial needling process, and can also reflect the hot melting process of the diaphragm under the condition of lower ohmic heat; the method has higher conformity with the actual conditions of the lithium ion battery, and can more accurately reflect the safety performance of the battery under the conditions of internal short circuit, needling and the like compared with the conventional test methods (such as DSC, thermal shrinkage and the like), thereby providing more reliable evidence for the design and material selection of the safety battery.
The steel needle is a high-temperature resistant steel needle, and the temperature or the heating rate of the steel needle can be controlled through the thermal resistance wire and the temperature probe.
Preferably, the diameter of the steel needle is 1-8 mm.
Preferably, the speed of the steel needle penetrating the septum is 0.01-30 mm/s.
The penetration of the septum by the steel needle described in the present invention includes two cases, the first case is:
preferably, the steel needle vertically penetrates through the diaphragm from top to bottom at a constant temperature of 20-500 ℃, and the standing time is kept to be more than 1 s;
further, the steel needle vertically penetrates through the diaphragm from top to bottom at a constant temperature of 25-300 ℃, and the standing time is kept to be more than 1 s; i.e. a steel needle penetrating the septum at a constant temperature.
The other situation is as follows:
preferably, the steel needle vertically penetrates through the diaphragm from top to bottom at a heating rate of 0.01-1 ℃/s, and the standing time is kept to be more than 1 s; i.e. the steel needle penetrates the septum at a rate of temperature increase.
Preferably, the detection method fixes the diaphragm between the positive pole piece and the negative pole piece through a clamp.
Preferably, round holes are reserved in the centers of the positive pole piece and the negative pole piece, and the diameter of each round hole is larger than that of the steel needle; the positive pole piece and the negative pole piece are the same in size, and the positions of the round holes are the same, namely the round holes are located at the centers of the positive pole piece and the negative pole piece.
Further, the positive pole piece and the negative pole piece can be electrode pieces obtained by disassembling the battery when a designed battery system is charged to different charge states; the size, formula, thickness and the like of the positive pole piece and the negative pole piece are the same as those of the designed battery system.
As a preferred technical solution of the present invention, the detection method comprises the following steps:
(1) fixing the diaphragm between the positive pole piece and the negative pole piece through a clamp; round holes are reserved in the centers of the positive pole piece and the negative pole piece, and the diameters of the round holes are larger than that of the steel needle;
(2) vertically penetrating the steel needle through the diaphragm from top to bottom at a speed of 0.01-30 mm/s and at a constant temperature of 25-300 ℃, and keeping standing for more than 1 s; the thermal resistance wire and the temperature probe are arranged in the steel needle, the conical angle of the needle point of the steel needle is 45-60 degrees, and the diameter of the steel needle is 1-8 mm.
As a preferred technical solution of the present invention, the detection method comprises the following steps:
(1) fixing the diaphragm between the positive pole piece and the negative pole piece through a clamp; round holes are reserved in the centers of the positive pole piece and the negative pole piece, and the diameters of the round holes are larger than that of the steel needle;
(2) vertically penetrating the steel needle through the diaphragm from top to bottom at a speed of 0.01-30 mm/s and a heating rate of 0.01-1 ℃/s, and keeping the standing time to be more than 1 s; the thermal resistance wire and the temperature probe are arranged in the steel needle, the conical angle of the needle point of the steel needle is 45-60 degrees, and the diameter of the steel needle is 1-8 mm.
Judging the short circuit safety of the diaphragm by detecting the deformation condition, the rupture condition and the broken hole area of the diaphragm after the detection is finished; the deformation condition refers to the extension condition of the diaphragm along with the steel needle and can be obtained by high-speed video playback; the rupture condition refers to the number of film cracks and the length of the cracks after the steel needle penetrates through the diaphragm; in addition, the size of the broken hole area of the diaphragm is calculated by using transparent coordinate paper.
The invention has the beneficial effects that:
(1) the detection method can obtain the damage condition of the diaphragm when the steel needle pierces the diaphragm under specific temperature (or temperature rise rate); when the temperature of the steel needle is equal to room temperature, the puncture strength can be obtained; meanwhile, the diaphragm with the optimal matching cost performance can be selected according to the damage condition of the diaphragm during detection at different temperatures (or temperature rise rates) and by combining the heat generation condition of a battery system.
(2) The invention clamps the diaphragm by the positive and negative pole pieces in the practical battery system, and the stress condition and the heat conduction condition of the diaphragm have high conformity with the practical condition.
(3) The change condition of the diaphragm along with temperature and force can be obtained simultaneously by the detection method.
Drawings
FIG. 1 is a schematic view of a pre-detection apparatus;
FIG. 2 is a schematic view of a detecting device in the detecting process of the present invention;
FIG. 3 is a schematic view of the inspection apparatus;
in the figure: 1. a positive electrode plate; 2. a diaphragm to be tested; 3. a negative pole piece; 4. a clamp; 5. a temperature probe; 6. a thermal resistance wire; 7. a steel needle; 8. a circular hole.
Detailed Description
The following examples are intended to illustrate the invention but are not intended to limit the scope of the invention.
The membranes to be tested in the examples are as follows:
A1: 20 μm wet PE-based film with 3 μm thick Al on both sides2O3Coating;
a2: 20 mu m PP/PE/PP composite basal membrane and double-sided ceramic 3 mu m Al respectively2O3Coating;
a3: 20 mu m PP dry method basal membrane and double-sided ceramic 3 mu m Al respectively2O3Coating;
a4: 26 mu m PET non-woven fabric base film/Al2O3Coating a composite membrane;
b1: 16 μm wet PE-based film with 3 μm thick Al on both sides2O3Coating;
b2: 20 mu m PP/PE/PP composite basal membrane and double-sided ceramic 5 mu m Al respectively2O3And (4) coating.
The detection method of the safety of the diaphragm comprises the following steps: the different types of diaphragms with the area of 144mm x 199mm are taken, fixed on a clamp together with high nickel/SiC system positive and negative electrode plates with the same size, and placed on a detection device (shown in figures 1-3).
The damaged area evaluating method comprises the following steps: after testing, flatly paving the diaphragm, and counting the defect area of the diaphragm by using transparent coordinate paper;
the tearing condition evaluating method comprises the following steps: tear hole number, tear hole length.
Example 1
The embodiment provides a method for detecting the safety of a lithium ion battery diaphragm, which comprises the following steps:
(1) 3A 1, A2, A3 and A4 diaphragms are taken and fixed between a positive pole piece and a negative pole piece through clamps respectively; round holes are reserved in the centers of the positive pole piece and the negative pole piece, and the diameters of the round holes are 8 mm;
(2) vertically penetrating the steel needle through the diaphragm from top to bottom at a speed of 6mm/s and at a constant temperature (60 ℃, 130 ℃ and 300 ℃ respectively), and keeping standing for 10 s; the thermal resistance wire and the temperature probe are arranged in the steel needle, the conical angle of the needle point of the steel needle is 45-60 degrees, and the diameter of the steel needle is 5 mm.
The present embodiment addresses the impact of the type of diaphragm substrate; the test results are averaged, and the damage condition of each diaphragm is shown in table 1;
TABLE 1 breakage of the A1, A2, A3, A4 septums
As can be seen from table 1, the thermal stability of the separator a4> A3> a2> a 1; the puncture strength of the septum is A1> A2> A3> A4.
Example 2
The embodiment provides a method for detecting the safety of a lithium ion battery diaphragm, which comprises the following steps:
(1) 3 diaphragms A1 and B1 are taken respectively, and are fixed between a positive pole piece and a negative pole piece through clamps; round holes are reserved in the centers of the positive pole piece and the negative pole piece, and the diameters of the round holes are 8 mm;
(2) vertically penetrating the steel needle through the diaphragm from top to bottom at a speed of 0.2mm/s and at a constant temperature (25 ℃ and 140 ℃ respectively), and keeping standing for 10 s; the thermal resistance wire and the temperature probe are arranged in the steel needle, the conical angle of the needle point of the steel needle is 45-60 degrees, and the diameter of the steel needle is 5 mm.
This example addresses the effect of the thickness of the diaphragm substrate; the test results are averaged, and the damage condition of each diaphragm is shown in table 2;
TABLE 2 breakage of the A1 and B1 diaphragms
As can be seen from table 2, the thermal stability of the separator a1> B1; the puncture strength of the septum a1> B1.
Example 3
The embodiment provides a method for detecting the safety of a lithium ion battery diaphragm, which comprises the following steps:
(1) 3 diaphragms A2 and B2 are taken respectively, and are fixed between a positive pole piece and a negative pole piece through clamps; round holes are reserved in the centers of the positive pole piece and the negative pole piece, and the diameters of the round holes are 8 mm;
(2) vertically penetrating the steel needle through the diaphragm from top to bottom at a rate of 30mm/s and at a constant temperature (40 ℃, 170 ℃ and 220 ℃ respectively), and keeping standing for 10 s; the thermal resistance wire and the temperature probe are arranged in the steel needle, the conical angle of the needle point of the steel needle is 45-60 degrees, and the diameter of the steel needle is 5 mm.
This example addresses the effect of ceramic coating thickness; the test results are averaged, and the breakage condition of each diaphragm is shown in table 3;
TABLE 3 breakage of the A2 and B2 diaphragms
As can be seen from table 3, the thermal stability of the separator, B2> a 2; the puncture strength of the septum B2> a 2.
Test example 1
In the test example, six separators A1, A2, A3, A4, B1 and B2 and an NCM/SiC battery system are assembled into batteries (the battery numbers are the same as those of the separators) with the capacities of 10Ah and 25Ah, and the needling safety condition of the batteries is evaluated, and the specific results are shown in Table 4;
TABLE 4 needling results for six separator composition batteries
Analysis of results
The detection results of comparative examples 1 to 3 show that the thermal stability of the separator is A4> A3> A2> A1, A1> B1, and B2> A2; the puncture strength of the septum is A1> A2> A3> A4, A1> B1, B2> A2;
as can be seen from table 4, both the thermal stability and the puncture strength of the separator are very important; when the thermal stability or the heat dissipation condition of the battery is good, the battery with high needling strength (such as A1 and B1) can inhibit the short circuit of a steel needle or control the short circuit area caused by mechanical damage at the initial stage of needling, thereby further reducing the heat generation; when the whole heat dissipation environment of the battery is poor (25Ah), the diaphragm with high thermal stability can relieve the further contraction condition of the diaphragm caused by the inertia temperature rise of the battery, slow down the spread of the internal short circuit caused by the diaphragm inside the battery, and further reduce the heat production rate.
In conclusion, the detection method has high reference significance for screening the high-needling safety diaphragm.
Although the invention has been described in detail hereinabove by way of general description, specific embodiments and experiments, it will be apparent to those skilled in the art that many modifications and improvements can be made thereto based on the invention. Accordingly, such modifications and improvements are intended to be within the scope of the invention as claimed.
Claims (10)
1. The method for detecting the safety of the lithium ion battery diaphragm is characterized by comprising the step of penetrating the diaphragm by a steel needle, wherein the speed of penetrating the diaphragm by the steel needle is 0.01-100 mm/s;
wherein, the steel needle is internally provided with a thermal resistance wire and a temperature probe, and the conical angle of the needle point of the steel needle is 45-60 degrees.
2. The detection method according to claim 1, wherein the diameter of the steel needle is 1-8 mm.
3. The detection method according to claim 1 or 2, wherein the rate of penetration of the steel needle through the septum is 0.01 to 30 mm/s.
4. The detection method according to any one of claims 1 to 3, wherein the steel needle penetrates the septum vertically from top to bottom at a constant temperature of 20 to 500 ℃ and is kept standing for more than 1 s.
5. The detection method according to claim 4, wherein the steel needle vertically penetrates the septum from top to bottom at a constant temperature of 25-300 ℃ and is kept standing for more than 1 s.
6. The detection method according to any one of claims 1 to 3, wherein the steel needle vertically penetrates the diaphragm from top to bottom at a heating rate of 0.01 to 1 ℃/s, and is kept standing for more than 1 s.
7. The detection method according to any one of claims 1 to 6, wherein the separator is fixed between the positive electrode sheet and the negative electrode sheet by a jig.
8. The detection method according to claim 7, wherein a round hole is reserved at the center of each of the positive electrode plate and the negative electrode plate, and the diameter of each round hole is larger than that of the steel needle.
9. The detection method according to claim 1, characterized by comprising the steps of:
(1) fixing the diaphragm between the positive pole piece and the negative pole piece through a clamp; round holes are reserved in the centers of the positive pole piece and the negative pole piece, and the diameters of the round holes are larger than that of the steel needle;
(2) vertically penetrating the steel needle through the diaphragm from top to bottom at a speed of 0.01-30 mm/s and at a constant temperature of 25-300 ℃, and keeping standing for more than 1 s; the thermal resistance wire and the temperature probe are arranged in the steel needle, the conical angle of the needle point of the steel needle is 45-60 degrees, and the diameter of the steel needle is 1-8 mm.
10. The detection method according to claim 1, characterized by comprising the steps of:
(1) fixing the diaphragm between the positive pole piece and the negative pole piece through a clamp; round holes are reserved in the centers of the positive pole piece and the negative pole piece, and the diameters of the round holes are larger than that of the steel needle;
(2) vertically penetrating the steel needle through the diaphragm from top to bottom at a speed of 0.01-30 mm/s and a heating rate of 0.01-1 ℃/s, and keeping the standing time to be more than 1 s; the thermal resistance wire and the temperature probe are arranged in the steel needle, the conical angle of the needle point of the steel needle is 45-60 degrees, and the diameter of the steel needle is 1-8 mm.
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| EP4105620A4 (en) * | 2020-12-17 | 2023-10-04 | LG Energy Solution, Ltd. | Device and method for evaluating heat resistance properties of separator |
| WO2023205967A1 (en) * | 2022-04-24 | 2023-11-02 | 宁德新能源科技有限公司 | Separator and device comprising same |
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