CN115436277A - Evaluation device and aging evaluation method - Google Patents
Evaluation device and aging evaluation method Download PDFInfo
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- CN115436277A CN115436277A CN202211026327.7A CN202211026327A CN115436277A CN 115436277 A CN115436277 A CN 115436277A CN 202211026327 A CN202211026327 A CN 202211026327A CN 115436277 A CN115436277 A CN 115436277A
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- 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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- G—PHYSICS
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
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Abstract
The invention discloses an evaluation device and an aging evaluation method, wherein the evaluation device comprises: the holding bottle is provided with a first opening and a second opening, the holding bottle is suitable for holding solution to simulate the chemical environment where an evaluation object is located, the sample assembly is placed in the holding bottle through the first opening, the sample is arranged in the sample space of the sample assembly, the tension rod of the pull-off assembly penetrates through the second opening, one end of the tension rod is connected to the sample assembly, and the tension rod applies tension to simulate the mechanical environment where the evaluation object is located. Therefore, on one hand, the aging evaluation test of the adhesive can be realized, and the blank in the industry is filled; more importantly, in the test process, the chemical environment and the mechanical environment can be simulated simultaneously, the test method is closer to a real use scene, and the evaluation precision and the evaluation accuracy can be improved.
Description
Technical Field
The present invention relates to the field of evaluation devices, and in particular, to an evaluation device and an aging evaluation method.
Background
In the related art, in the conventional carbon fiber material field, the lithium battery technical field and the like, aging evaluation is performed on the material and the like of the product, however, the aging evaluation is generally directed to the structure of the product itself, for example: carbon cloth, graphite, diaphragms, and the like.
However, the aging evaluation of the adhesive between the adjacent carbon cloth layers, the adjacent plates, and the structural members cannot be performed effectively, the aging of the adhesive also affects the service life, reliability, and the like of the product, and it is difficult to achieve the synchronous simulation of the chemical environment and the mechanical environment in the testing process.
Disclosure of Invention
The present invention is directed to solving at least one of the problems of the prior art. Therefore, an object of the present invention is to provide an evaluation device, which can simulate a chemical environment and a mechanical environment, and can realize aging evaluation of an adhesive with more accurate evaluation results, thereby filling the gap in the industry.
The invention further provides an aging evaluation method adopting the evaluation device.
An evaluation apparatus according to an embodiment of the first aspect of the present invention includes: the container bottle is provided with a first opening and a second opening, the container bottle is suitable for containing solution to simulate the chemical environment of an assessment object, the sample assembly is placed in the container bottle through the first opening, a sample is arranged in the sample space of the sample assembly, a tension rod of the pull-off assembly penetrates through the second opening, one end of the tension rod is connected to the sample assembly, and the tension rod applies tension to simulate the mechanical environment of the assessment object.
According to the evaluation device provided by the embodiment of the invention, on one hand, the aging evaluation test of the adhesive can be realized, and the blank in the industry is filled; more importantly, in the test process, the chemical environment and the mechanical environment can be simulated at the same time, the real use scene is closer, and the evaluation precision and the evaluation accuracy can be improved.
According to some embodiments of the invention, the containment bottle comprises: the sample assembly comprises a bottle body, a first bottle stopper and a second bottle stopper, wherein one end of the bottle body is provided with a first opening, a first bottle stopper cover is arranged at the first opening, the side direction of the bottle body is provided with a second opening, a second bottle stopper cover is arranged at the second opening, a fixing part is arranged at the bottom of the bottle body and on the first bottle stopper, and the fixing part is used for fixing the sample assembly. From this, through setting up the fixed part to set up first bottle plug, second bottle plug respectively on first opening and second opening, on the one hand, the sealing performance of holding the bottle is better, higher corrosion resistance has, can satisfy the solution injection that has certain corrosivity, improve application scope, on the other hand, sample subassembly and holding the bottle realization can dismantle the cooperation, but sample subassembly cyclic utilization, and the change of sample is simple, convenient, can reduce cost, improve efficiency of software testing, reduce the test degree of difficulty.
In some embodiments, a sealing element is arranged between the second opening and the tension rod, so that the solution in the bottle body can be effectively prevented from overflowing, and the reliability and safety of the evaluation device in the evaluation and test processes are improved.
According to some embodiments of the invention, the sample assembly comprises: the device comprises a first plate and a second plate which are oppositely arranged, wherein a sample space is arranged between the first plate and the second plate, a sample is prepared in the sample space, the tension rod is connected with the second plate, and the first plate is connected with the containing bottle.
That is to say, after the pull-off test, the sample breaks away from with first board and/or second board in step, and the dismantlement between sample and the sample subassembly is simpler, convenient, and can used repeatedly after accomplishing the dismantlement, also can reduce test cost.
Furthermore, the first plate or the second plate is further provided with a plurality of clamping grooves extending along the length direction and the width direction of the sample assembly, the baffle is detachably arranged in the clamping grooves, the sample space with an open opening is limited by the baffle, the first plate and the second plate, the preparation difficulty of the sample can be reduced, after the sample is prepared, the sample can be simultaneously bonded with the first plate and the second plate, the process of assembling the sample to the sample space after the sample is prepared is omitted, the testing steps are simplified, the testing efficiency is improved, the volume of the sample space can be limited to be kept constant, the sample with the same volume can be prepared, the repeatability and the reliability of the test and the experiment are improved, and the sample assembly is more reliable
Furthermore, the one end of pull rod is provided with the sucking disc, and through the sucking disc with the second board links to each other, can make pull rod and second board realize that the structure that links to each other is simpler, and the operation that both link to each other is simpler, convenient.
Furthermore, one end of the tension rod is provided with a first fastener, the second plate is provided with a second fastener, and the first fastener is in threaded fit with the second fastener, so that the tension rod is connected with the second plate. Like this, realize being connected through screw-thread fit, can improve the connection stability of pull rod and second board, avoid among the test procedure, the second board breaks away from the cooperation with the pull rod.
According to some embodiments of the invention, the first plate and the second plate are arranged in groups, and the first plate and the second plate of each group are made of the same material. Thus, the first plate and the second plate can be made of aluminum plates, copper plates, stainless steel plates and the like, can be adapted to different samples, and can increase the application range of the evaluation device.
Further, the first opening is located in a first direction, the second opening is located in a second direction, and the first direction is orthogonal to the second direction. Therefore, the assembly direction is orthogonal to the pull-off direction, vertical pull-off can be achieved, the pulling force in the pull-off test process does not need to be converted into vertical pulling force, the pull-off test precision is higher, and the evaluation effect is more accurate.
The aging evaluation method according to the embodiment of the second aspect of the present invention, which employs the above evaluation apparatus, includes:
preparing a sample;
placing the sample and the sample assembly in the containing bottle, and injecting electrolyte;
and applying a first pulling force through the pulling rod, maintaining the first time length, releasing the pulling rod, maintaining the second time length, repeating for multiple times until the sample is stripped from the sample assembly, and recording the stripping time, wherein the first time length is the same as the second time length.
According to the evaluation method provided by the embodiment of the invention, the stripping test is carried out by adopting the tension applying process, the stripping time is in positive correlation with the aging of the adhesive, the longer the stripping time is, the longer the service life of the corresponding adhesive is, the shorter the aging time is, the shorter the stripping time is, the shorter the service life of the corresponding adhesive is, and the shorter the aging time is, and in the stripping time test, the sample is positioned in a containing bottle with electrolyte, so that the chemical environment can be simulated, the stripping time accuracy is improved, and the evaluation effect accuracy is improved.
Further, the preparing the sample comprises:
injecting a sample liquid into the sample space;
baking the sample assembly at the first temperature for a third time period to obtain the dried sample.
Further, the aging evaluation method further includes:
obtaining a sample component mass W while preparing a sample 1 Total mass W of said sample assembly and said sample 2 And calculating the mass W of the sample 0 ＝W 2 -W 1 ；
Obtaining a current sample mass W after the sample is peeled off the sample assembly 3 To obtain a swelling ratio R = (W) 3 -W 0 )/W 0 ×100％。
Further, the aging evaluation method further includes:
after the swelling ratio is obtained, baking the sample at the second temperature for a fourth time to obtain the current sample mass W 4 To obtain a dissolution rate C = (W) W -W 4 )/W 0 ×100％。
Additional aspects and advantages of the invention will be set forth in part in the description which follows and, in part, will be obvious from the description, or may be learned by practice of the invention.
Drawings
The above and/or additional aspects and advantages of the present invention will become apparent and readily appreciated from the following description of the embodiments, taken in conjunction with the accompanying drawings of which:
FIG. 1 is a schematic view of an evaluation device according to an embodiment of the invention;
FIG. 2 is a schematic view of a containment vial according to an embodiment of the present invention;
FIG. 3 is a schematic view of a sample assembly according to an embodiment of the invention;
FIG. 4 is a schematic view of a pull-off assembly according to an embodiment of the present invention;
FIG. 5 is a schematic view of a first plate according to an embodiment of the invention;
FIG. 6 is a flow diagram of a method of aging evaluation according to an embodiment of the present invention.
Reference numerals:
the evaluation device 100 is provided with a display device,
a containing bottle 10, a bottle body 11, a first opening 111, a second opening 112, a first bottle stopper 12, a second bottle stopper 13, a fixing portion 14,
a pull-off assembly 30, a tension bar 31, a suction cup 32,
a seal 40.
Detailed Description
Reference will now be made in detail to embodiments of the present invention, examples of which are illustrated in the accompanying drawings, wherein like or similar reference numerals refer to the same or similar elements or elements having the same or similar function throughout. The embodiments described below with reference to the accompanying drawings are illustrative only for the purpose of explaining the present invention, and are not to be construed as limiting the present invention.
The evaluation apparatus 100 and the aging evaluation method according to the embodiment of the present invention are described below with reference to fig. 1 to 6.
As shown in fig. 1 to 5, an evaluation apparatus 100 according to an embodiment of the first aspect of the present invention includes: housing vial 10, sample assembly 20, and pull-off assembly 30.
The holding bottle 10 has a first opening 111 and a second opening 112, the holding bottle 10 is suitable for holding a solution to simulate a chemical environment where an evaluation object is located, the sample assembly 20 is placed in the holding bottle 10 through the first opening 111, the sample is disposed in a sample space of the sample assembly 20, the pull rod 31 of the pull-off assembly 30 penetrates through the second opening 112, and one end of the pull rod 31 is connected to the sample assembly 20, and the pull rod 31 applies a pulling force to simulate a mechanical environment where the evaluation object is located.
It should be noted that the sample space of the sample assembly 20 of the embodiment of the present invention can be used for accommodating a plate-like or strip-like structure, so that the evaluation device 100 of the present invention can be used for at least the aging evaluation of an adhesive, a pole piece, and the like.
It is understood that an evaluator refers to a product to which a sample corresponds, and the sample may be an entire product or a portion of a product, such as: pole pieces of lithium ion batteries, adhesives, and the like.
Specifically, the sample is arranged in the sample assembly 20, the pulling-off rod of the pulling-off assembly 30 acts on the sample assembly 20, so that the pulling-off rod can pull the sample assembly 20 to simulate a mechanical environment, and the solution can be injected into the containing bottle 10 to simulate a chemical environment, so that the mechanical environment and the chemical environment of the sample are closer to those of a product, and the evaluation precision can be effectively improved.
Furthermore, the length of time taken for the pulling-off assembly 30 to peel off the sample, and the physical quantities such as quality change generated before and after peeling off the sample can be used as experimental data for aging evaluation, specifically represent or embody product characteristics such as aging information, impedance, low temperature resistance, suitability with chemical liquid in a use scene, and the like, so that various performances of the tested sample can be evaluated conveniently.
Illustratively, the test of the adhesive can be performed by the evaluation apparatus 100, the test of the peeling can be performed by the pull-off assembly 30, and the test of the dissolution rate, the swelling rate, and the like can be performed by the injection of the solution, and the test of the sheet member of the pole piece can be performed by the evaluation apparatus 100, and the test of the peeling, the dissolution rate, the swelling rate, and the like can be included.
According to the evaluation device 100 of the embodiment of the invention, on one hand, the aging evaluation test of the adhesive can be realized, and the blank in the industry is filled; more importantly, in the test process, the chemical environment and the mechanical environment can be simulated simultaneously, the test method is closer to a real use scene, and the evaluation precision and the evaluation accuracy can be improved.
Preferably, the first opening 111 is located in a first direction, and the second opening 112 is located in a second direction, the first direction being orthogonal to the second direction. Therefore, the assembling direction is orthogonal to the pulling-out direction, vertical pulling-out can be achieved, the pulling force in the pulling-out test process does not need to be converted into vertical pulling force, the pulling-out test precision is higher, and the evaluation effect is more accurate.
As shown in fig. 2, according to some embodiments of the present invention, containment bottle 10 comprises: the bottle comprises a bottle body 11, a first bottle stopper 12 and a second bottle stopper 13, wherein a first opening 111 is formed in one end of the bottle body 11, the first bottle stopper 12 is arranged on the first opening 111 in a covering mode, a second opening 112 is formed in the lateral direction of the bottle body 11, the second bottle stopper 13 is arranged on the second opening 112 in a covering mode, fixing portions 14 are arranged on the bottom of the bottle body 11 and the first bottle stopper 12, and the fixing portions 14 are used for fixing a sample assembly 20.
Specifically, the containing bottle 10 is used as a container capable of containing a solution, and in order to match with the real use environment of a product (i.e., an evaluation object) corresponding to a sample to be measured, the bottle body 11, the first bottle stopper 12 and the second bottle stopper 13 can be made of polytetrafluoroethylene materials or aluminum alloy materials with compact oxide layers, so that the corrosion resistance is good, and liquids with certain corrosiveness, such as electrolyte, can be contained to simulate a chemical environment.
Furthermore, by positioning the first opening 111 and the second opening 112 in the first direction and the second direction, respectively, the pull-off assembly 30 and the sample assembly 20 can be prevented from being assembled; or before the test, interference is generated in the preparation process, the first bottle stopper 12 and the second bottle stopper 13 may be configured to be in threaded connection, insertion connection, and the like with the bottle body 11, and in order to avoid the solution in the bottle body 11 from overflowing, the second bottle stopper 13 located on the lateral side (second direction) of the bottle body 11 needs to be sealed to ensure that the solution does not overflow while passing through the sample, and the first bottle stopper 12 should be sealed correspondingly according to the characteristics of the injected solution, such as volatility of the injected solution.
It should be pointed out that, fixed part 14 is two, forms respectively on the diapire of first bottle stopper 12 and bottle 11, and two fixed part 14 set up relatively, and two fixed part 14 can all be constructed slot, jack structure to make sample subassembly 20 detachably set up in holding bottle 10, be convenient for change the sample in the sample space, with the aassessment test of carrying out different samples, make sample subassembly 20 circulated use, and reduce cost, and the change of sample in the sample space is simple, convenient, reduces the test degree of difficulty.
That is to say, through setting up fixed part 14 to set up first bottle plug 12, second bottle plug 13 on first opening 111 and second opening 112 respectively, on the one hand, the sealing performance of holding bottle 10 is better, has higher corrosion resistance, can satisfy the solution injection that has certain corrosivity, improve application scope, on the other hand, sample subassembly 20 realizes dismantling the cooperation with holding bottle 10, sample subassembly 20 circulated use, and the change of sample is simple, and is convenient, can reduce cost, improve efficiency of software testing, reduce the test degree of difficulty.
As shown in fig. 1, in some embodiments, a seal 40 is disposed between the second opening 112 and the tension rod 31.
It should be noted that the second opening 112 is located at the lateral side of the bottle body 11, in order to simulate a chemical environment, the solution in the container bottle 10 at least needs to submerge the sample, the sample is located above the second opening 112, in order to avoid the solution overflowing, a sealing member 40 needs to be arranged on the second opening 112, if a sealing arrangement is adopted between the second bottle stopper 13 and the second opening 112, the tension rod 31 penetrates through the second bottle stopper 13, the sealing member 40 is arranged on an area, which is required to be arranged on the second bottle stopper 13 for the tension rod 31 to penetrate through, and if a sealing arrangement is not adopted between the second bottle stopper 13 and the second opening 112, two sealing members 40 need to be arranged to respectively realize the sealing between the second bottle stopper 13 and the second opening 112, and the sealing between the tension rod 31 and the second bottle stopper 13; or one sealing member 40 simultaneously achieves sealing between the second stopper 13 and the second opening 112, and the tension rod 31 and the second stopper 13.
Therefore, the solution in the bottle body 11 can be effectively prevented from overflowing, and the reliability and the safety of the evaluation device 100 in the evaluation and test processes can be improved.
As shown in fig. 3, according to some embodiments of the present invention, the sample assembly 20 includes: the first plate 21 and the second plate 22 are oppositely arranged, a sample space is arranged between the first plate 21 and the second plate 22, a sample is prepared to the sample space, the tension rod 31 is connected with the second plate 22, and the first plate 21 is connected with the containing bottle 10.
Specifically, the first plate 21 and the second plate 22 are oppositely arranged in the second direction, the first plate 21 is spaced from the second plate 22, at least part of the spaced region forms a sample space, a sample is prepared in the sample space, and in the preparation process, the sample is bonded with the first plate 21 and the second plate 22, so that the first plate 21 is fixed in the accommodating bottle 10 through the fixing part 14, the second plate 22 is connected with the tension rod 31, the tension rod 31 pulls the second plate 22, a pulling force is continuously provided to act on the second plate 22, and the continuously provided pulling force can be kept constant for a long time; changes over time; or repeatedly switching between two or more tension values, and the like, until the first plate 21 and the sample and/or the second plate 22 are disengaged from the sample, namely, completing the pull-off test, wherein the pull-off test result can be peeling under the action of large tension (peeling tension) or peeling after the pull is performed for a long time (peeling duration).
That is to say, after the pull-off test is finished, the sample is synchronously separated from the first plate 21 and/or the second plate 22, the disassembly between the sample and the sample assembly 20 is simpler and more convenient, the sample can be repeatedly used after the disassembly is finished, and the test cost can also be reduced.
As shown in fig. 3 and 5, a plurality of clamping grooves 23 extending in the length direction and the width direction of the sample assembly 20 are further provided on the first plate 21 or the second plate 22, a blocking plate 24 is detachably provided on the clamping grooves 23, and the blocking plate 24, the first plate 21, and the second plate 22 define a sample space having one open opening.
The card slot 23 may include two first card slots 23 and two second card slots 23 extending along the length direction of the sample assembly 20, and a third card slot 23 extending along the width direction of the sample assembly 20 and intersecting the first card slot 23 and the second card slot 23; or the clamping groove 23 may include two first clamping grooves 23 and two second clamping grooves 23 extending along the width direction of the sample assembly 20, and one third clamping groove 23 extending along the length direction of the sample assembly 20 and intersecting with the first clamping groove 23 and the second clamping groove 23, so as to define a sample space with an open opening by the baffles 24, the first plate 21 and the second plate 22 arranged in the clamping grooves 23, the sample may be injected into the sample space through the open opening in an injection manner, after the sample is formed, and after the sample is formed, the three baffles 24 may be respectively drawn out from the corresponding clamping grooves 23, so as to complete the preparation of the sample, reduce the difficulty in the preparation of the sample, and may define that the volume of the sample space is kept constant, so as to prepare samples with the same volume, thereby increasing the repeatability and reliability of tests and experiments.
It can be understood that the sample of the present invention is directly prepared in the sample space between the first plate 21 and the second plate 22, injected through the open port, and after the sample preparation is completed, the sample is simultaneously bonded to the first plate 21 and the second plate 22, so that the process of assembling the sample to the sample space after the sample preparation is omitted, the testing steps are simplified, and the testing efficiency is improved.
As shown in fig. 4, in some embodiments, the tension rod 31 is provided with a suction cup 32 at one end thereof and is connected to the second plate 22 through the suction cup 32. From this, the pull rod 31 links to each other through vacuum actuation form with the second board 22, and pull rod 31 pulling sucking disc 32, sucking disc 32 pulling second board 22 are in order to realize exerting the pulling force to sample subassembly 20, and the structure that makes pull rod 31 and second board 22 realize linking to each other is simpler, and the operation that both link to each other is simpler, convenient.
Of course, the form of the connection between the tension rod 31 and the second plate 22 according to the embodiment of the present invention is not limited to this, and in other embodiments, a first fastening member is disposed at one end of the tension rod 31, a second fastening member is disposed on the second plate 22, and the first fastening member is in threaded engagement with the second fastening member, so that the tension rod 31 is connected to the second plate 22, that is, the second plate 22 is connected to the tension rod 31 through a threaded structure, the first fastening member is formed as a nut, and the second fastening member is formed as an external thread at one end of the tension rod 31, and the connection is achieved through threaded engagement, so that the connection stability between the tension rod 31 and the second plate 22 can be improved, and the second plate 22 and the tension rod 31 are prevented from being disengaged during the test.
According to some embodiments of the present invention, the first plate 21 and the second plate 22 are disposed in groups, and the material of the first plate 21 and the second plate 22 in each group is the same.
Specifically, the first plate 21 and the second plate 22 may each be made of an aluminum plate, a copper plate, a stainless steel plate, or the like, and the applicability of the evaluation apparatus 100 of the present invention may be increased to adapt to different samples. For example, when preparing a negative electrode binder sample of a lithium ion battery, the first plate 21 and the second plate 22 should be made of copper plates, when preparing a positive electrode binder sample of a lithium ion battery, the first plate 21 and the second plate 22 should be made of aluminum plates, and when performing relevant tests on pole pieces of a lithium ion battery, the materials of the first plate 21 and the second plate 22 are not particularly limited.
As shown in fig. 6, according to the aging evaluation method according to the embodiment of the second aspect of the present invention, the aging evaluation method using the above evaluation apparatus 100 includes:
preparing a sample;
placing the sample and the sample assembly 20 in the containing bottle 10, and injecting electrolyte;
applying a first pulling force through the tension bar 31 for a first duration, releasing the tension bar 31, maintaining for a second duration, and repeating a plurality of times until the sample is peeled from the sample assembly 20, and recording the peel time, wherein the first duration is the same as the second duration.
Illustratively, after preparing the sample, the sample and sample assembly 20 is placed into the bottle 11 through the first opening 111, the first plate 21 is fixed by the two fixing portions 14, and the electrolyte is injected, after the tension bar 31 is connected to the second plate 22, a tension of 5N/m is applied, after 30min is maintained, the tension bar is released, so that the tension is reduced to 0N/m and maintained for 30min, and the above steps are repeated for recording time until the first plate 21 and/or the second plate 22 is separated from the sample, the peeling test is completed, and the peeling time is recorded.
According to the evaluation method provided by the embodiment of the invention, the stripping test is carried out by adopting the tension applying process, the stripping time is in positive correlation with the aging of the adhesive, the longer the stripping time is, the longer the service life of the corresponding adhesive is, the shorter the aging time is, the shorter the stripping time is, the shorter the service life of the corresponding adhesive is, and the shorter the aging time is, and in the stripping time test, the sample is positioned in the containing bottle 10 with the electrolyte, so that the chemical environment can be simulated, the stripping time accuracy is improved, and the evaluation effect accuracy is improved.
Further, preparing the sample comprises:
injecting a sample liquid into the sample space;
the sample assembly 20 is baked at the first temperature for a third period of time to obtain a baked sample.
Therefore, the sample is prepared by injecting the liquid material, and the sample is cured by baking in the preparation process, so that the sample preparation process is simple and reliable, and the cost is low.
As shown in fig. 5, the aging evaluation method further includes:
in preparing the sample, a sample assembly 20 mass W is obtained 1 Total mass W of sample assembly 20 and sample 2 And calculating the mass W of the sample 0 ＝W 2 -W 1 ；
After the sample is stripped from the sample assembly 20, the current sample mass W is taken 3 To obtain a swelling ratio R = (W) 3 -W 0 )/W 0 ×100％；
After the swelling rate is obtained, baking the sample at the second temperature for a fourth time period to obtain the current sample mass W 4 To obtain a dissolution rate C = (W) 0 -W 4 )/W 0 ×100％。
Therefore, the dissolution rate and the swelling rate of the sample can be obtained, and when the test sample is a binder, a pole piece and the like of a lithium battery, the swelling rate is closely related to the impedance and the low temperature of the lithium battery; the dissolution rate is closely related to the corrosion resistance of the adhesive and the pole piece, and can be used for evaluating the adaptability of the electrolyte and the adhesive and predicting the cycle life of the lithium ion battery, and generally, the higher the dissolution rate is, the poorer the matching performance of the adhesive and the electrolyte is, and the shorter the cycle life is.
With reference to fig. 6, a specific process of evaluating a pole piece, a positive electrode binder or a negative electrode binder of a lithium ion battery by using the evaluation method of the present invention is described as follows:
first, it should be noted that the flowchart shown in fig. 6 is summarized, the solid open arrows indicate the step processes of the test process, the solid arrows indicate the processes of acquiring the physical quantities, and the solid arrows indicate the processes of calculating.
1. Preparation of samples
Before the preparation of the sample is started, the clamping groove 23 on the first plate 21 needs to be baked for 8 hours at 80 ℃ to remove moisture, and then the weight W1 of the sample assembly 20 is obtained by weighing;
the positive electrode binder may be prepared by using aluminum plates as the first plate 21 and the second plate 22, wherein the surface tension of the aluminum plates is close to that of an aluminum foil used in the lithium ion battery, preparing the positive electrode binder into a 10% solid glue solution, injecting the glue solution into a sample space by using a syringe, baking the sample space at 90 ℃ for 12 hours to obtain a sample, weighing the sample to obtain a total mass W2 of the sample assembly 20 and the sample, and withdrawing the baffle 24 to obtain the sample, wherein the weight W0= W2-W1 of the sample.
The negative electrode binder sample was prepared as above except that the first plate 21 and the second plate 22 are preferably copper plates;
the preparation method of the positive and negative pole pieces is the same as the above, except that the material injected into the sample space is the slurry for producing the lithium battery rather than the adhesive liquid.
2. Test procedure
As shown in fig. 1, the storage bottle 10 is a wide-mouth bottle, the first plate 21 of the sample assembly 20 can be inserted into the fixing portion 14 at the bottom of the bottle body 11 by opening the first opening 111, and the suction cup 32 of the pull-off assembly 30 or the assembly of the first fastener and the second fastener can provide a stable pulling force, after the installation is completed, electrolyte is injected, the current time T1 is recorded, 5N/m pulling force is applied, after 30min is maintained, the pulling force is reduced to 0N/m and maintained for 30min, and this is repeated for a plurality of times until the first plate 21 or the second plate 22 and the sample (positive electrode adhesive sample, negative electrode adhesive sample or positive electrode plate sample) are peeled off, and the time T2 is recorded, and the peeling time T = T2-T1 is obtained by the following formula;
taking out the stripped sample, wiping the surface electrolyte with dust-free paper, and weighing to obtain the current sample mass W 3 The swelling ratio R = (W) was calculated by the following equation 3 -W 0 )/W 0 ×100％；
Baking the sample at 90 ℃ for 8 hours, and weighing to obtain the current sample weight W 4 The dissolution rate C = (W) is calculated by the following formula 0 -W 4 )/W 0 ×100％。
3. Analysis of results
By the evaluation apparatus 100 and the evaluation method of the present invention, tests of the swelling ratio, the peeling time, and the dissolution rate can be simultaneously realized. Generally, the stripping time is closely related to the aging of the adhesive film, and the longer the stripping time is, the longer the aging time is, the longer the service life is; the swelling ratio is closely related to the impedance and low temperature of the lithium battery; the dissolution rate is closely related to the electrolyte resistance of the adhesive film, and can be used for evaluating the adaptability of the electrolyte and the binder and predicting the cycle life of the lithium ion battery, and generally, the higher the dissolution rate is, the poorer the matching between the binder and the electrolyte is, and the shorter the cycle life is.
Therefore, the evaluation device 100 and the evaluation method can supplement the blank that the binder cannot be tested in the industry, have accurate test results, and are convenient for aging analysis, impedance, low temperature, the matching of the binder and the electrolyte, the cycle life and the like.
In the description of the present invention, it is to be understood that the terms "central," "longitudinal," "lateral," "length," "width," "thickness," "upper," "lower," "front," "rear," "left," "right," "vertical," "horizontal," "top," "bottom," "inner," "outer," "clockwise," "counterclockwise," "axial," "radial," "circumferential," and the like are used in the orientations and positional relationships indicated in the drawings for convenience in describing the invention and to simplify the description, and are not intended to indicate or imply that the referenced device or element must have a particular orientation, be constructed and operated in a particular orientation, and are not to be considered limiting of the invention.
In the description of the present invention, "the first feature" and "the second feature" may include one or more of the features.
In the description of the present invention, "a plurality" means two or more.
In the description of the invention, "on" or "under" a first feature may include that the first and second features are in direct contact, and may also include that the first and second features are not in direct contact but are in contact via another feature between them.
In the description of the invention, "above", "over" and "above" a first feature in a second feature includes the first feature being directly above and obliquely above the second feature, or simply means that the first feature is higher in level than the second feature.
In the description herein, references to the description of the term "one embodiment," "some embodiments," "an illustrative embodiment," "an example," "a specific example," or "some examples" or the like mean that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the invention. In this specification, the schematic representations of the terms used above do not necessarily refer to the same embodiment or example. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples.
While embodiments of the invention have been shown and described, it will be understood by those of ordinary skill in the art that: various changes, modifications, substitutions and alterations can be made to the embodiments without departing from the principles and spirit of the invention, the scope of which is defined by the claims and their equivalents.
Claims (13)
1. An evaluation device, comprising:
a containment vial having a first opening and a second opening, the containment vial adapted to contain a solution therein to simulate a chemical environment in which the analyte is located;
a sample assembly placed in the containment vial through the first opening, a sample disposed in a sample space of the sample assembly;
and the tension rod of the pull-off assembly penetrates through the second opening, one end of the tension rod is connected to the sample assembly, and tension is applied through the tension rod to simulate the mechanical environment of the evaluation object.
2. The evaluation device of claim 1, wherein the containment vial comprises: the sample assembly comprises a bottle body, a first bottle stopper and a second bottle stopper, wherein one end of the bottle body is provided with a first opening, a first bottle stopper cover is arranged at the first opening, the side direction of the bottle body is provided with a second opening, a second bottle stopper cover is arranged at the second opening, a fixing part is arranged at the bottom of the bottle body and on the first bottle stopper, and the fixing part is used for fixing the sample assembly.
3. The evaluation device of claim 2, wherein a seal is disposed between the second opening and the tension rod.
4. The evaluation device of claim 1, wherein the sample assembly comprises: the device comprises a first plate and a second plate which are oppositely arranged, wherein a sample space is arranged between the first plate and the second plate, a sample is prepared in the sample space, the tension rod is connected with the second plate, and the first plate is connected with the containing bottle.
5. The evaluation device according to claim 4, wherein the first plate or the second plate is further provided with a plurality of catching grooves extending in a length direction and a width direction of the sample assembly, a blocking plate is detachably provided to the catching grooves, and the blocking plate, the first plate and the second plate define the sample space having one opening.
6. The evaluation device according to claim 4, wherein the one end of the tension bar is provided with a suction cup and is connected to the second plate through the suction cup.
7. The evaluation device of claim 4, wherein the one end of the tension bar is provided with a first fastener and the second plate is provided with a second fastener, the first fastener being threadably engaged with the second fastener to couple the tension bar to the second plate.
8. The device according to any one of claims 4 to 7, wherein the first and second plates are arranged in groups, and wherein the first and second plates of each group are of the same material.
9. The evaluation device of claim 1, wherein the first opening is located in a first direction and the second opening is located in a second direction, the first direction being orthogonal to the second direction.
10. An aging evaluation method that employs the above evaluation apparatus, characterized by comprising:
preparing a sample;
placing the sample and the sample assembly in the containing bottle, and injecting electrolyte;
and applying a first pulling force through the pulling rod, maintaining the first time length, releasing the pulling rod, maintaining the second time length, repeating the steps for multiple times until the sample is stripped from the sample assembly, and recording the stripping time, wherein the first time length is the same as the second time length.
11. The aging evaluation method according to claim 10, wherein the preparing a sample includes:
injecting a sample liquid into the sample space;
baking the sample assembly at the first temperature for a third time period to obtain the dried sample.
12. The aging evaluation method according to claim 10, further comprising:
obtaining a sample component mass W while preparing a sample 1 Total mass W of said sample assembly and said sample 2 And calculating the mass W of the sample 0 ＝W 2 -W 1 ；
Obtaining a current sample mass W after the sample is peeled off the sample assembly 3 To obtain a swelling ratio R = (W) 3 -W 0 )/W 0 ×100％。
13. The aging evaluation method according to claim 12, further comprising:
in what is obtainedAfter the swelling rate is obtained, baking the sample at the second temperature for a fourth time to obtain the current sample mass W 4 To obtain a dissolution rate C = (W) 0 -W 4 )/W 0 ×100％。
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