CN113358559A - Test method for evaluating actual adhesion effect of gluing diaphragm - Google Patents
Test method for evaluating actual adhesion effect of gluing diaphragm Download PDFInfo
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- 238000010998 test method Methods 0.000 title claims abstract description 24
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- 238000012360 testing method Methods 0.000 claims abstract description 40
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N19/00—Investigating materials by mechanical methods
- G01N19/04—Measuring adhesive force between materials, e.g. of sealing tape, of coating
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Abstract
The invention relates to a test method for evaluating the actual adhesion effect of a gluing diaphragm, which comprises the following steps: (1) stacking at least one group of the pole piece, the gluing diaphragm and the isolating layer which are sequentially stacked, and hot-pressing; (2) the hot-pressed sample was subjected to a peel force test. The testing method is simple and easy to operate, and can evaluate the actual adhesion effect of the gluing diaphragm.
Description
Technical Field
The invention relates to the technical field of lithium ion batteries, in particular to a test method for evaluating the actual adhesion effect of a gluing diaphragm.
Background
In a lithium ion battery, the primary function of a separator is to keep the positive and negative electrodes separated to prevent short circuits, while allowing rapid transfer of ions, which is an important component in a lithium ion battery. The performance of the separator directly affects the characteristics of the battery, such as the capacity, internal resistance, rate, cycle and self-discharge of the battery, and particularly, the safety is important.
The separator, referred to as the "third pole" of the lithium battery, serves to prevent physical contact of the electrodes and allows free conduction of ions. Currently, the separator materials used in commercial liquid lithium ion batteries are mainly microporous polyolefin thin films, such as single-layer or multi-layer composite films of Polyethylene (PE) and polypropylene (PP). As a diaphragm substrate, the PE/PP can provide good mechanical property and chemical stability, has a high-temperature self-closing characteristic, and can ensure the safety of the lithium ion battery to a certain extent. However, as the application of the lithium ion battery in the fields of electric vehicles, energy storage and the like is continuously extended, higher indexes are provided for the performance of each key material forming the battery. In order to improve the safety of the battery, at present, a power battery enterprise widely uses a functional diaphragm, and tries to improve the safety of the battery on the basis of not influencing the electrochemical performance of the battery.
The innovation of the diaphragm technology is also rapidly developed, the glue-coated diaphragm is the most promising at the present stage, and the introduction of the glue-coated diaphragm can effectively solve the problems of the wrinkle of the pole piece interface of the square aluminum shell battery, the lithium precipitation and the battery cycle. The action mechanism of the gluing diaphragm is that the pole piece is influenced by repeated expansion of the active material as little as possible in the charging and discharging process through the adhesion of the glue, so that the wrinkles of the pole piece are reduced, and the long cycle performance is improved. An important criterion for a rubberized separator, therefore, is its adhesion to the pole piece interface. Current peel force testing for rubberized membranes is primarily focused between the coating and the base film.
CN105606529A discloses a method for testing the peel strength of a coated membrane of a lithium ion battery, which comprises the steps of preparing a glue joint sample by bonding the coating surface of the coated membrane with a glass slide by an adhesive, reversing the coated membrane by 180 degrees, peeling the glue joint sample from an opening of the glue joint by a universal tensile testing machine at a specified speed, so that the coated membrane is gradually separated from the glass slide along the length direction of the bonded surface, the coating of the coated membrane is completely bonded from a base membrane by the adhesive in the separation process, so that the coating is separated from the base membrane, and the force value of the coating automatically obtained by the testing machine when the coating is separated from the base membrane is calculated according to the force value, so as to calculate the peel strength between the coated membrane and the base membrane. However, the peeling strength test method for the gluing diaphragm disclosed by the method aims at the peeling strength between the coating and the base film, but because the adhesion force of the gluing layer is different among different materials, the peeling strength between the coating and the base film can not visually reflect the performances of the gluing diaphragm and the pole piece in practical use only by testing, and the using effect of the gluing diaphragm can only be checked by disassembling after the battery is assembled, so that the test period is greatly prolonged, and unnecessary time cost and labor and material cost are increased.
CN110132842A discloses a method for detecting the adhesion strength of a lithium ion battery coating membrane, which mainly comprises the steps of preparing a test sample strip, assembling the test sample strip, detecting the test sample strip and calculating the result. However, in the test method disclosed by the method, the test sample strip is firstly adhered to the steel plate during sample preparation, the sample can be prepared into a single layer during hot pressing, the adhesion between the adhesive-coated diaphragm and the pole piece is obviously changed along with the increase of the number of winding layers in an actual winding core, and the real situation of the diaphragm cannot be accurately reflected by a single-layer test sample.
In conclusion, it is important to develop a test method which is simple to operate and can evaluate the actual adhesion effect of the gluing membrane.
Disclosure of Invention
Aiming at the defects of the prior art, the invention aims to provide a test method for evaluating the actual adhesion effect of a gluing membrane, which is simple and easy to operate and can evaluate the actual adhesion effect of the gluing membrane.
In order to achieve the purpose, the invention adopts the following technical scheme:
the invention provides a test method for evaluating the actual adhesion effect of a gluing diaphragm, which comprises the following steps:
(1) stacking at least one group (such as two groups, three groups, five groups, ten groups, fifteen groups, twenty-five groups, thirty-five groups, forty-five groups and the like) of the pole pieces, the gluing diaphragms and the isolating layers which are sequentially stacked, and carrying out hot pressing;
(2) the hot-pressed sample was subjected to a peel force test.
According to the invention, the gluing diaphragm and the pole piece are laminated and then are subjected to hot pressing, so that the adhesion force of the diaphragm in the winding core when the diaphragm is in contact with the pole piece is simulated, and the expression of the gluing diaphragm in different winding layer numbers of the actual winding core can be reflected more truly; according to different gluing diaphragm application products, the pole pieces of the winding cores of corresponding models are adopted, the number of stacked layers can be freely increased according to the required conditions, the measuring mode is more flexible, and the using effect of the gluing diaphragm in different products can be reflected more pertinently; in addition, the invention does not need to judge the adhesive effect of the adhesive coating diaphragm by disassembling the observation interface after the battery is completely off-line, and only needs simple lamination hot pressing, thereby greatly shortening the analysis period of the product service condition and saving a large amount of cost.
Preferably, the number of the sets of the pole pieces, the adhesive-coated membranes and the isolation layers which are sequentially stacked in step (1) is one to fifty, such as two, three, five, ten, fifteen, twenty-five, thirty-five, forty-five, etc.
Preferably, the pressure of the hot pressing in step (1) is 3.5-9.5t, such as 4t, 5t, 5.5t, 6t, 6.5t, 7t, 7.5t, 8t, 8.5t, 9t, etc. The reason for controlling the pressure of the hot pressing in this range is that when the pressure is too low, the gluing membrane cannot be well bonded with the pole piece layer, and when the pressure is too high, the active material layer on the pole piece is damaged, so that the test result is affected.
Preferably, the temperature of the hot pressing is 60-95 ℃, such as 65 ℃, 70 ℃, 75 ℃, 80 ℃, 85 ℃, 90 ℃ and the like. The reason for controlling the hot-pressing temperature within this range is that the adhesive layer needs to reach a certain temperature for adhesion, and the excessive temperature may cause the membrane to shrink to a certain extent, which affects the adhesion effect.
Preferably, the hot pressing time is 30-90s, such as 35s, 40s, 45s, 50s, 55s, 60s, 65s, 70s, 75s, 80s, 85s, etc. The reason for controlling the time of the hot pressing within this range is similar to the reason for controlling the pressure and temperature ranges, both for better exerting the adhesive effect of the rubberized membranes.
Preferably, the step (1) specifically comprises: the pole pieces, the adhesive-coated separator, and the separator, which are sequentially stacked, are stacked in at least one set (e.g., two, three, five, ten, fifteen, twenty-five, thirty-five, forty-five, fifty-five, etc.), and hot-pressed for 30 to 90s (e.g., 35s, 40s, 45s, 50s, 55s, 60s, 65s, 70s, 75s, 80s, 85s, 90s, etc.) under a pressure of 3.5 to 9.5t (e.g., 4t, 5t, 5.5t, 6t, 6.5t, 7t, 7.5t, 8t, 8.5t, 9t, etc.) and a temperature of 60 to 95 ℃ (e.g., 65 ℃, 70 ℃, 75 ℃, 80 ℃, 85 ℃, etc.), to obtain a hot-pressed sample.
Preferably, before the sample is subjected to the peel force test in step (2), the method further comprises: and cutting the sample to obtain a cut sample.
Preferably, the length of the cut sample is 200-350mm, such as 220mm, 240mm, 260mm, 280mm, 300mm, 320mm, 340mm, etc.
Preferably, the width of the cut sample is 10-30mm, such as 12mm, 14mm, 16mm, 18mm, 20mm, 22mm, 24mm, 26mm, 28mm, and the like.
Preferably, the peel force test comprises the steps of: and arranging the sample on a substrate, poking the adjacent gluing diaphragms and pole pieces, and folding to finish the test of the stripping force.
Preferably, the substrate comprises a stainless steel plate.
Preferably, the sample is arranged on the substrate in an adhesive manner, and the side of the sample, which is not in contact with the gluing membrane, of the pole piece is close to the substrate.
Preferably, the bonding means is double-sided adhesive bonding.
Preferably, the bonding specifically comprises the steps of: and adhering a double-sided adhesive tape to the substrate, and adhering the sample to the double-sided adhesive tape to complete adhesion.
Preferably, the double-sided adhesive is adhered to the substrate and then rolled.
Preferably, the number of rolling is 1-3, such as 1, 2, 3, etc.
Preferably, the sample is stuck on the double-sided adhesive and then comprises a rolling operation.
Preferably, the number of rolling is 2-4, such as 2, 3, 4, etc.
Preferably, in the peel force test, the direction for separating the adjacent diaphragm from the pole piece is along the long side of the diaphragm and the pole piece.
Preferably, the length of the kick-off is 10-30mm, such as 12mm, 14mm, 16mm, 18mm, 20mm, 22mm, 24mm, 26mm, 28mm, and the like.
Preferably, the means for testing the peel force comprises a peel force tester.
Preferably, the step (2) specifically comprises: cutting the sample obtained in the step (1), wherein the length of the cut sample is 200-350mm (for example, 220mm, 240mm, 260mm, 280mm, 300mm, 320mm, 340mm and the like), the width of the cut sample is 10-30mm (for example, 12mm, 14mm, 16mm, 18mm, 20mm, 22mm, 24mm, 26mm, 28mm and the like), then adhering the double-sided adhesive on a substrate, rolling for 1-3 times (for example, 1 time, 2 times, 3 times and the like), then adhering the cut sample on the double-sided adhesive, rolling for 2-4 times (for example, 2 times, 3 times, 4 times and the like), completing adhesion, and then pulling apart the adjacent diaphragm and the pole piece in the adhered sample by 10-30mm (for example, 12mm, 14mm, 16mm, 18mm, 20mm, 22mm, 24mm, 26mm, 28mm and the like) along the long edge of the pole piece, and completing the test of the peeling force.
As a preferred technical solution, the testing method comprises the following steps:
(1') stacking at least one group of the pole piece, the gluing diaphragm and the isolating layer which are sequentially stacked, and carrying out hot pressing for 30-90s under the conditions that the pressure is 3.5-9.5t and the temperature is 60-95 ℃ to obtain a hot-pressed sample;
(2') cutting the sample obtained in the step (1'), wherein the length of the cut sample is 200-350mm, and the width of the cut sample is 10-30mm, then adhering the double-sided adhesive on a substrate of a peeling force tester, rolling for 1-3 times, adhering the cut sample on the double-sided adhesive, and rolling for 2-4 times to complete adhesion, so as to obtain an adhered sample;
(3') poking the adjacent diaphragm and the pole piece in the sample obtained in the step (2') for 10-30mm along the long edge, and turning over to finish the test of the peeling force.
Compared with the prior art, the invention has the following beneficial effects:
(1) according to the invention, the gluing diaphragm and the pole piece are laminated and then are hot-pressed, so that the adhesion force of the diaphragm in the winding core when the diaphragm is in contact with the pole piece is simulated, the expression of the gluing diaphragm in different winding layers of the actual winding core can be reflected more truly, and the stripping force is reduced from the upper layer to the lower layer along with the increase of the hot-pressing layer; under different hot pressing conditions, the corresponding stripping force value is changed;
(2) according to the invention, the pole pieces of the roll cores with corresponding models are adopted according to different gluing diaphragm application products, the number of stacked layers can be freely increased according to the required conditions, the measuring mode is more flexible, and the using effect of the gluing diaphragm in different products can be reflected more pertinently;
(3) according to the method, after the battery is completely off-line, the adhesive effect of the adhesive coating diaphragm is judged by disassembling the observation interface, and only simple lamination hot pressing is needed, so that the analysis period of the product use condition is greatly shortened, a large amount of cost is saved, the mean value change of the peeling strength is 0-0.2N/m, and the mean value change rate is within 8.9%.
Drawings
FIG. 1 is a schematic structural view of a sample after completion of bonding as described in the test method described in example 1;
wherein, 1-an isolating layer; 2-gluing a diaphragm; 3-pole piece, 4-substrate.
Detailed Description
For the purpose of facilitating an understanding of the present invention, the present invention will now be described by way of examples. It should be understood by those skilled in the art that the examples are only for the understanding of the present invention and should not be construed as the specific limitations of the present invention.
Example 1
The embodiment provides a test method for evaluating the actual adhesion effect of a gluing membrane, which comprises the following steps:
(1) sequentially laminating three groups of pole pieces 3 (positive pole piece with the thickness of 163 μm), a gluing diaphragm 2 (ceramic diaphragm with the thickness of 9 μm and double-sided coating and the thickness of 1 μm) and an isolating layer 1(A4 paper) in sequence, and carrying out hot pressing for 60s under the conditions that the pressure is 6.5t and the temperature is 85 ℃ to obtain a hot-pressed sample;
(2) cutting the sample obtained in the step (1), wherein the cut sample is a sample strip with the length of 270mm and the width of 30mm, adhering a double-faced adhesive to a substrate 4 (a stainless steel plate) of a peeling force tester, rolling for 1 time, adhering the cut sample to the double-faced adhesive, and rolling for 3 times to complete adhesion, so as to obtain an adhered sample, wherein the specific structure diagram is shown in fig. 1;
(3) and placing the bonded sample in a testing area, poking the adjacent diaphragm and the pole piece for 30mm along the long edge under the action of a chuck, and folding the diaphragm in the stretching direction of the chuck to finish the test of the peeling force.
Example 2
The difference between this example and example 1 is that the electrode piece is a negative electrode piece (the thickness of the electrode piece is 119 μm), and the rest is the same as example 1.
Example 3
The embodiment provides a test method for evaluating the actual adhesion effect of a gluing membrane, which comprises the following steps:
(1) sequentially laminating fifteen groups of pole pieces (positive pole piece, thickness of 172 μm), a gluing diaphragm (ceramic diaphragm, thickness of 9 μm, double-sided coating, coating thickness of 2 μm) and an isolating layer (A4 paper) in sequence, and carrying out hot pressing for 30s under the conditions of pressure of 6t and temperature of 85 ℃ to obtain a hot-pressed sample;
(2) cutting the sample obtained in the step (1), wherein the length is 300mm and the width is 25mm, adhering a double-sided adhesive tape on a substrate (stainless steel plate) of a peeling force tester, rolling for 2 times, adhering the cut sample on the double-sided adhesive tape, and rolling for 4 times to complete adhesion, so as to obtain an adhered sample;
(3) and placing the bonded sample in a testing area, poking the adjacent diaphragm and the pole piece for 30mm along the long edge under the action of a chuck, and folding the diaphragm in the stretching direction of the chuck to finish the test of the peeling force.
Examples 4 to 5
Examples 4 to 5 are different from example 1 in that the hot pressing pressures were 7.5t and 8.5t, respectively, and the rest was the same as example 1.
Examples 6 to 7
Examples 6 to 7 are different from example 2 in that the hot pressing pressures were 7.5t and 8.5t, respectively, and the rest was the same as example 2.
Comparative examples 1 to 2
Comparative examples 1-2 differ from examples 1-2 in that cores having the same number of pole pieces, adhesive coated separator and separator layers and the same hot pressing conditions were subjected to the peel force test.
Comparative example 3
Comparative example 3 differs from example 3 in that the cores having the same number of pole pieces, adhesive coated separator and separator layers and the same hot pressing conditions were subjected to the peel force test.
Comparative examples 4 to 5
Comparative examples 4-5 differ from examples 4-5 in that cores having the same number of pole pieces, adhesive coated separator and separator layers and the same hot pressing conditions were subjected to the peel force test.
Comparative examples 6 to 7
Comparative examples 6-7 differ from examples 6-7 in that cores having the same number of pole pieces, adhesive coated separator and separator layers and the same hot pressing conditions were subjected to the peel force test.
Performance testing
The peel strength between adjacent pole pieces and adhesive-coated membranes in examples 1-7 and comparative examples 1-7 was tested in whole or in part according to the test method described above, where the number of groups of pole pieces, adhesive-coated membranes, and separator layers increased from top to bottom as the number of stacked layers in hot pressing, and the test results are summarized in tables 1-2.
TABLE 1
TABLE 2
In Table 1, examples 3-4 and comparative examples 3-4 tested the peel strength of the pole pieces from the rubberized membranes in groups 11-13, and the remaining examples and comparative examples tested the peel strength of the pole pieces from the rubberized membranes in groups 1-3.
As can be seen from the analysis of the data in Table 1, in the results of the seven groups of peel strengths described above, example 1 and comparative example 1, example 2 and comparative example 2, example 3 and comparative example 3, example 4 and comparative example 4, example 5 and comparative example 5, example 6 and comparative example 6, example 7 and comparative example 7, the peel strength values corresponding to the separator and the peel strength values of the same group of electrode sheets and the gummed separator are close, and the peel strength values of the adjacent three groups are also close, the specific data are shown in Table 2, the mean change value of the peel strength is calculated by the absolute value of the difference between the mean values of the peel strengths of the examples and the comparative examples, the mean change rate is the ratio of the corresponding mean change value to the peel strength of the examples, the mean change of the peel strength is between 0 and 0.2N/m, and the mean change rate is within 8.9%, which proves that the test method of the invention can effectively evaluate the actual adhesion effect of the gummed separator, and the operation is simple and repeatable.
The applicant states that the present invention is illustrated in detail by the above examples, but the present invention is not limited to the above detailed methods, i.e. it is not meant that the present invention must rely on the above detailed methods for its implementation. It should be understood by those skilled in the art that any modification of the present invention, equivalent substitutions of the raw materials of the product of the present invention, addition of auxiliary components, selection of specific modes, etc., are within the scope and disclosure of the present invention.
Claims (10)
1. A test method for evaluating the actual adhesion effect of a glued membrane is characterized by comprising the following steps:
(1) stacking at least one group of the pole piece, the gluing diaphragm and the isolating layer which are sequentially stacked, and hot-pressing;
(2) the hot-pressed sample was subjected to a peel force test.
2. The test method for evaluating the actual adhesion effect of the rubberized membrane according to claim 1, wherein the number of the sets of the pole pieces, the rubberized membranes and the isolation layers which are sequentially stacked in the step (1) is one to fifty sets.
3. A test method for evaluating the actual adhesion of a rubberized membrane according to claim 1 or 2, characterized in that the pressure of said hot pressing in step (1) is comprised between 3.5 and 9.5 t;
preferably, the temperature of the hot pressing is 60-95 ℃;
preferably, the time for the hot pressing is 30-90 s.
4. A test method for evaluating the actual adhesion of a rubberized membrane according to any one of claims 1 to 3, characterised in that said step (1) comprises in particular: and stacking at least one group of the pole piece, the gluing diaphragm and the isolating layer which are sequentially stacked, and carrying out hot pressing for 30-90s under the conditions that the pressure is 3.5-9.5t and the temperature is 60-95 ℃ to obtain a hot-pressed sample.
5. A test method for evaluating the actual adhesion of a rubberized membrane according to any one of claims 1 to 4, wherein said sample in step (2) is further subjected, before being subjected to a peel force test, to: cutting the sample to obtain a cut sample;
preferably, the length of the cut sample is 200-350 mm;
preferably, the width of the cut sample is 10-30 mm.
6. Test method for evaluating the actual adhesion of a rubberized membrane according to any one of claims 1 to 5, characterised in that said test of peel force comprises the following steps: arranging the sample on a substrate, poking the adjacent gluing diaphragms and pole pieces, and folding to finish the test of the stripping force;
preferably, the substrate comprises a stainless steel plate;
preferably, the sample is arranged on the substrate in a bonding mode, and the side, which is not contacted with the gluing membrane, of the pole piece in the sample is close to the substrate;
preferably, the bonding means is double-sided adhesive bonding.
7. Test method for evaluating the actual adhesion of a rubberized membrane according to claim 6, characterised in that said adhesion comprises in particular the steps of: adhering a double-sided adhesive tape to a substrate, and adhering the sample to the double-sided adhesive tape to complete adhesion;
preferably, the double-sided adhesive is adhered to the substrate and then rolled;
preferably, the number of rolling is 1 to 3;
preferably, the sample is stuck on the double-sided adhesive and then comprises the operation of rolling;
preferably, the number of rolling is 2 to 4.
8. A test method for evaluating the actual adhesion effect of a rubberized membrane according to any one of claims 1 to 7, wherein, in the peel force test, the direction of separating the adjacent membrane from the pole piece is along the long sides of the membrane and the pole piece;
preferably, the length of the poke is 10-30 mm;
preferably, the means for testing the peel force comprises a peel force tester.
9. Test method for evaluating the actual adhesion of a rubberized membrane according to any one of claims 1 to 8, characterised in that said step (2) comprises in particular: cutting the sample obtained in the step (1), wherein the length of the cut sample is 200-350mm, and the width of the cut sample is 10-30mm, adhering a double-sided adhesive on a substrate, rolling for 1-3 times, adhering the cut sample on the double-sided adhesive, rolling for 2-4 times to complete adhesion, poking the adjacent diaphragm and pole piece in the adhered sample for 10-30mm along the long edge, and turning over to complete the test of the stripping force.
10. Test method for evaluating the actual adhesion of a rubberized membrane according to any one of claims 1 to 9, characterised in that it comprises the following steps:
(1') stacking at least one group of the pole piece, the gluing diaphragm and the isolating layer which are sequentially stacked, and carrying out hot pressing for 30-90s under the conditions that the pressure is 3.5-9.5t and the temperature is 60-95 ℃ to obtain a hot-pressed sample;
(2') cutting the sample obtained in the step (1'), wherein the length of the cut sample is 200-350mm, and the width of the cut sample is 10-30mm, then adhering the double-sided adhesive on a substrate of a peeling force tester, rolling for 1-3 times, adhering the cut sample on the double-sided adhesive, and rolling for 2-4 times to complete adhesion, so as to obtain an adhered sample;
(3') poking the adjacent diaphragm and the pole piece in the sample obtained in the step (2') for 10-30mm along the long edge, and turning over to finish the test of the peeling force.
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
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Application publication date: 20210907 |