CN113029866A - Electrolyte infiltration testing method and application thereof - Google Patents
Electrolyte infiltration testing method and application thereof Download PDFInfo
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- CN113029866A CN113029866A CN202110208905.8A CN202110208905A CN113029866A CN 113029866 A CN113029866 A CN 113029866A CN 202110208905 A CN202110208905 A CN 202110208905A CN 113029866 A CN113029866 A CN 113029866A
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N13/00—Investigating surface or boundary effects, e.g. wetting power; Investigating diffusion effects; Analysing materials by determining surface, boundary, or diffusion effects
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N5/00—Analysing materials by weighing, e.g. weighing small particles separated from a gas or liquid
Abstract
The invention provides an electrolyte infiltration testing method and application thereof, wherein the testing method comprises the following steps: taking a standard pole piece and a detection battery prepared by adopting the standard pole piece, dripping electrolyte on the standard pole piece and drying, and respectively weighing the weight of the standard pole piece before dripping the electrolyte, the quality of the dried standard pole piece and the dripping amount of the electrolyte; the method comprises the following steps of disassembling a working detection battery, disassembling a pole piece in the detection battery to be the detection pole piece, cutting the detection pole piece into at least two cutting blocks, airing and weighing the cutting blocks in sequence, cleaning and drying the cutting blocks in sequence after weighing, weighing the cutting blocks again after drying, and obtaining the infiltration parameters of the detection pole piece. The invention obtains the electrolyte infiltration conditions of different positions of the pole piece under different working states by taking the infiltration parameters of the standard pole piece as the basis, and has the characteristics of simple test method, low cost, accurate measurement result and the like.
Description
Technical Field
The invention belongs to the technical field of lithium ion batteries, and particularly relates to an electrolyte infiltration testing method and application thereof.
Background
The lithium ion battery has the advantages of high energy density, long service life, high rated voltage, low self-discharge rate, light first-level weight and the like, and is widely applied to the fields of mobile phones, notebook computers, electric vehicles and the like. The lithium ion battery comprises a positive electrode, a diaphragm, a negative electrode, electrolyte and a battery shell, wherein the electrolyte is an ion conductor which plays a role in conduction between the positive electrode and the negative electrode of the battery and transmits lithium ions in the charging and discharging process. The electrolyte has great influence on the charge and discharge performance, the rate capability, the high and low temperature performance, the cycle life, the calendar life and the like of the battery.
When the electrolyte infiltration effect is poor, the ion transmission path becomes far, so that the shuttle of lithium ions between the positive electrode and the negative electrode is hindered, the pole piece which is not contacted with the electrolyte cannot participate in the electrochemical reaction of the battery, and meanwhile, the interface resistance of the battery is increased, so that the multiplying power performance, the discharge capacity and the service life of the lithium battery are influenced.
At present, the two main electrolyte wettability testing methods are as follows, wherein one method is to observe the impregnation process of the electrolyte in the soft package battery by adopting a neutron imaging diffraction technology. The method utilizes the strong absorption effect of the electrolyte on neutrons to detect the process of the electrolyte infiltrating in the lithium ion battery, and has the problem of high test cost. Secondly, under the inert atmosphere, the suspension type balance is utilized to test the weight change of the pole piece for the adsorption and infiltration of the electrolyte, so as to test the infiltration performance of the pole piece, but only the infiltration performance of a fresh pole piece or a pole group for the electrolyte can be tested, and the infiltration condition of the electrolyte can not be tested under different conditions of soft package and square shell.
CN112084627A discloses a method for qualitatively characterizing wettability of electrolyte, comprising the following steps: s1, arranging a reference electrode between the positive electrode and the negative electrode of the battery cell to be injected to form a three-electrode system; s2, injecting electrolyte into the battery cell to be injected, and measuring the impedance of the positive electrode to the reference electrode and the impedance of the negative electrode to the reference electrode at intervals after sealing to obtain impedance diagrams of the positive electrode and the negative electrode to the reference electrode; and S3, judging whether the electrolyte completely wets the anode material and the cathode material according to whether the ion impedance value in the impedance diagram changes. However, the method cannot determine the infiltration condition of different positions of the pole piece.
CN110487665A discloses a method for detecting wettability of a pole piece, which comprises the following steps: s1, pole piece pretreatment: coating a polyvinylidene fluoride layer on the surface of the pole piece to obtain a pole piece to be detected; s2, detecting wettability: and immersing the pole piece to be tested into the electrolyte, and calculating the infiltration speed according to the mass of the electrolyte entering the pole piece to be tested within a certain time. The method comprises the steps of coating a vinylidene fluoride layer on the surface of a pole piece, immersing the pole piece into electrolyte, and calculating the infiltration speed according to the mass of the electrolyte entering the pole piece to be tested within a certain time, so as to test the infiltration of the pole piece, but the infiltration distribution condition of the electrolyte cannot be measured.
The existing wettability measuring methods all have the problems of complex process, high cost and incapability of measuring the distribution condition of wettability, so how to measure the wettability of different positions of a pole piece under the condition of ensuring that the wettability measuring method is convenient to operate and low in cost becomes a problem which needs to be solved urgently at present.
Disclosure of Invention
Aiming at the defects in the prior art, the invention aims to provide an electrolyte infiltration testing method and application thereof.
In order to achieve the purpose, the invention adopts the following technical scheme:
in a first aspect, the present invention provides an electrolyte infiltration testing method, which comprises the following steps:
taking a standard pole piece and a detection battery prepared by adopting the standard pole piece, dripping electrolyte on the standard pole piece and drying, and respectively weighing the weight of the standard pole piece before dripping the electrolyte, the quality of the dried standard pole piece and the dripping amount of the electrolyte;
the method comprises the following steps of disassembling a working detection battery, disassembling a pole piece in the detection battery to be the detection pole piece, cutting the detection pole piece into at least two cutting blocks, airing and weighing the cutting blocks in sequence, cleaning and drying the cutting blocks in sequence after weighing, weighing the cutting blocks again after drying, and obtaining the infiltration parameters of the detection pole piece.
The invention tests the wettability of the electrolyte by a quality difference method, determines the wettability of the pole piece to the electrolyte by combining the quality of non-volatile substances in the electrolyte, obtains the conditions of electrolyte wettability at different positions in the detected pole piece based on the wettability parameters of a standard pole piece, analyzes the difference of the wettability of the pole piece to the electrolyte, and can determine the wettability of the pole piece to the electrolyte only by analyzing the test data of the standard pole piece. The invention can measure the batteries in different working states and has the characteristics of simple test method, low cost, accurate measurement result and the like.
It should be noted that the invention does not make specific requirements and special limitations on the types of pole pieces, and those skilled in the art can reasonably select the pole pieces according to the types of pole pieces in the battery to be tested, for example, the pole pieces are positive pole pieces and/or negative pole pieces.
It should be noted that the material of the electrolyte is not specifically required or limited, and those skilled in the art can reasonably select the material of the electrolyte according to the measurement requirement, for example, the electrolyte includes lithium hexafluorophosphate.
As a preferred technical solution of the present invention, the testing method specifically includes the following steps:
taking a standard pole piece and a detection battery prepared by adopting the standard pole piece, and weighing the standard pole piece to be m1The dropping quality of the standard pole piece is recorded as m2The electrolyte is dried to a stable quality, and the weight of the pole piece is weighed again and recorded as m3；
(II) disassembling the working detection battery, taking out the detection pole piece and cutting at least two cutting blocks, weighing the mass of the cutting blocks after the cutting blocks are dried and recording the mass as m4；
(III) cleaning the cut blocks with a cleaning agent, drying the cleaned cut blocks, weighing the cut blocks again after drying, and recording the mass m of the cut blocks5And calculating to obtain the infiltration parameters of the detection pole piece.
It should be noted that the material of the cleaning agent is not specifically required or limited, and the cleaning agent capable of cleaning the electrolyte on the electrode plate can be used in the present invention, and those skilled in the art can reasonably select the cleaning agent according to the kind of the electrolyte, for example, the cleaning agent is dimethyl carbonate.
As a preferable technical scheme of the invention, in the step (I), the injection standard is 0.8-3 g/g, for example, the injection standard is 0.8g/g, 1.0g/g, 1.2g/g, 1.4g/g, 1.6g/g, 1.8g/g, 2.0g/g, 2.2g/g, 2.4g/g, 2.6g/g, 2.8g/g or 3.0 g/g.
It should be noted that the liquid injection standard is the electrolyte quality required by the battery pole group per unit mass, which meets the design requirements of the battery, and the parameters vary with the design requirements of the battery cell, and those skilled in the art can reasonably select the liquid injection standard according to the design requirements of the battery cell.
As a preferred technical scheme of the invention, in the step (I), the pole piece is dripped with electrolyte under a dry environment.
Preferably, the humidity of the dry environment is < 10%, e.g., the humidity is 1%, 2%, 3%, 4%, 5%, 6%, 7%, 8%, or 9%.
As a preferable technical scheme of the invention, in the step (II), the pole piece is divided into a center cutting area, a transition cutting area and an edge cutting area along the center to the edge, and the cutting block is respectively cut in the center cutting area, the transition cutting area and the edge cutting area.
Preferably, the center cutting area, the transition cutting area and the edge cutting area are arranged in a concentric circle or a concentric matrix at the center of the pole piece.
Preferably, the radius of the central cutting area, the loop width of the transition cutting area and the loop width of the edge cutting area are equal.
As a preferred technical scheme of the invention, in the step (III), the infiltration parameters comprise unit mass electrolyte infiltration amount of the standard pole piece, infiltration electrolyte content of different positions of the detected pole piece and unit mass electrolyte infiltration amount of different positions of the detected pole piece.
As one preferable aspect of the present inventionAccording to the technical scheme, the infiltration capacity of the electrolyte per unit mass of the standard pole piece is marked as AStandard of meritSaid A isStandard of merit＝m2/m1。
As a preferred technical scheme of the invention, the content of the electrolyte infiltrated at different positions of the detection pole piece is recorded as mAnalysis ofM is saidAnalysis of＝(m4-m5)*m2/(m3-m1)。
As a preferred technical scheme of the invention, the unit mass electrolyte infiltration capacity of different positions of the detection pole piece is marked as AAnalysis ofSaid A isAnalysis of＝mAnalysis of/m5。
Exemplarily, the method for testing the electrolyte infiltration includes the following steps:
taking a standard pole piece and a detection battery prepared by adopting the standard pole piece, and weighing the standard pole piece to be m1And under the dry environment with the humidity less than 10%, the dropping quality of the standard pole piece is recorded as m2The electrolyte is injected to the liquid injection standard of 0.8-3 g/g, and after the standard pole piece is dried to be stable in quality, the weight of the pole piece is weighed again and recorded as m3；
(II) disassembling the working detection battery, taking out the detection pole piece and cutting at least two cutting blocks, weighing the mass of the cutting blocks after the cutting blocks are dried and recording the mass as m4；
(III) cleaning the cut blocks with a cleaning agent, drying the cleaned cut blocks, weighing the cut blocks again after drying, and recording the mass m of the cut blocks5And calculating to obtain the infiltration parameters of the detection pole piece.
In a second aspect, the present invention further provides a use of the electrolyte infiltration test method according to the first aspect, where the electrolyte infiltration test method is used for measuring electrolyte infiltration in a lithium ion battery.
The recitation of numerical ranges herein includes not only the above-recited numerical values, but also any numerical values between non-recited numerical ranges, and is not intended to be exhaustive or to limit the invention to the precise numerical values encompassed within the range for brevity and clarity.
Compared with the prior art, the invention has the beneficial effects that:
the invention tests the wettability of the electrolyte by a quality difference method, determines the wettability of the pole piece to the electrolyte by combining the quality of non-volatile substances in the electrolyte, obtains the conditions of electrolyte wettability at different positions in the detected pole piece based on the wettability parameters of a standard pole piece, analyzes the difference of the wettability of the pole piece to the electrolyte, and can determine the wettability of the pole piece to the electrolyte only by analyzing the test data of the standard pole piece. The method has the characteristics of simple test method, low cost, accurate measurement result and the like.
Drawings
FIG. 1 is a schematic diagram of the cutting of the positive and negative electrode plates in examples 1 to 3 of the present invention;
FIG. 2 is a graph showing the results of the test in example 1 of the present invention;
FIG. 3 is a graph showing the results of the test in example 2 of the present invention;
FIG. 4 is a graph showing the test results in example 3 of the present invention.
Wherein, 1-a central cutting area; 2-a transition cutting area; 3-edge cutting area.
Detailed Description
In order to better illustrate the present invention and facilitate the understanding of the technical solutions of the present invention, the present invention is further described in detail below. However, the following examples are only simple examples of the present invention and do not represent or limit the scope of the present invention, which is defined by the claims.
The technical solution of the present invention is further explained by the following embodiments.
Example 1
The embodiment provides an electrolyte infiltration testing method, which specifically comprises the following steps:
taking a standard pole piece and a detection battery prepared by adopting the standard pole piece, and weighing the standard pole piece to be m1Dropping the solution into the standard pole piece under the dry environment with the humidity less than 10 percentThe quantity is recorded as m2The electrolyte is dried to a stable quality, and the weight of the pole piece is weighed again and recorded as m3；
(II) after will work detect the battery and disassemble, take out and detect the pole piece and cut out two piece at least cutting off pieces, along the center of pole piece to the edge, as shown in figure 1, cutting off piece cuts respectively in the center cutting district 1 that is concentric rectangle with the pole piece center and arranges, transition cutting district 2 and edge cutting district 3, the radius in center cutting district 1, the ring width in transition cutting district 2 and the ring width in edge cutting district 3 equal, the cutting off piece is weighed after drying and is cut off the quality of piece and is recorded as m4；
(III) cleaning the cut blocks with a cleaning agent, drying the cleaned cut blocks, weighing the cut blocks again after drying, and recording the mass m of the cut blocks5And calculating to obtain the infiltration parameters of the detection pole piece.
The method is adopted to respectively carry out electrolyte infiltration tests on the positive pole piece and the negative pole piece, the electrolyte comprises lithium hexafluorophosphate, the cleaning agent is dimethyl carbonate, the infiltration flow of the detection battery is constant temperature standing for 2 hours at 45 ℃, and the test result is shown in figure 2:
in the negative electrode sheet, AStandard of merit0.78 g/g; a of the center cutting area 1Analysis of0.32 g/g; a of transition cutting area 2Analysis of0.54 g/g; a of the edge trimming area 3Analysis ofIt was 0.75 g/g.
In the positive electrode sheet, AStandard of merit0.40 g/g; a of the center cutting area 1Analysis of0.15 g/g; a of transition cutting area 2Analysis of0.27 g/g; a of the edge trimming area 3Analysis ofIt was 0.38 g/g.
Example 2
The embodiment provides an electrolyte infiltration testing method, which specifically comprises the following steps:
taking a standard pole piece and a detection battery prepared by adopting the standard pole piece, and weighing the standard pole piece to be m1And under the dry environment with the humidity less than 10%, the dropping quality of the standard pole piece is recorded as m2To the injection of electrolyteStandard, the liquid injection standard is 1.5g/g, after the standard pole piece is dried to be stable in quality, the weight of the pole piece is weighed again and recorded as m3；
(II) after will work detect the battery and disassemble, take out and detect the pole piece and cut out two piece at least cutting off pieces, along the center of pole piece to the edge, as shown in figure 1, cutting off piece cuts respectively in the center cutting district 1 that is concentric rectangle with the pole piece center and arranges, transition cutting district 2 and edge cutting district 3, the radius in center cutting district 1, the ring width in transition cutting district 2 and the ring width in edge cutting district 3 equal, the cutting off piece is weighed after drying and is cut off the quality of piece and is recorded as m4；
(III) cleaning the cut blocks with a cleaning agent, drying the cleaned cut blocks, weighing the cut blocks again after drying, and recording the mass m of the cut blocks5And calculating to obtain the infiltration parameters of the detection pole piece.
The method is adopted to respectively carry out electrolyte infiltration tests on the positive pole piece and the negative pole piece, the electrolyte comprises lithium hexafluorophosphate, the cleaning agent is dimethyl carbonate, the infiltration flow of the detection battery is constant temperature standing for 2 hours at 45 ℃, and the test result is shown in figure 3:
in the negative electrode sheet, AStandard of merit1.22 g/g; a of the center cutting area 1Analysis of0.79 g/g; a of transition cutting area 2Analysis of1.00 g/g; a of the edge trimming area 3Analysis ofIt was 1.19 g/g.
In the positive electrode sheet, AStandard of merit0.61 g/g; a of the center cutting area 1Analysis of0.39 g/g; a of transition cutting area 2Analysis of0.49 g/g; a of the edge trimming area 3Analysis ofIt was 0.59 g/g.
Example 3
The embodiment provides an electrolyte infiltration testing method, which specifically comprises the following steps:
taking a standard pole piece and a detection battery prepared by adopting the standard pole piece, and weighing the standard pole piece to be m1And under the dry environment with the humidity less than 10%, the dropping quality of the standard pole piece is recorded as m2The electrolyte is in a liquid injection standard of 3g/g, and the standard pole pieceAfter the pole piece is dried to be stable in quality, the weight of the pole piece is weighed again and recorded as m3；
(II) after will work detect the battery and disassemble, take out and detect the pole piece and cut out two piece at least cutting off pieces, along the center of pole piece to the edge, as shown in figure 1, cutting off piece cuts respectively in the center cutting district 1 that is concentric rectangle with the pole piece center and arranges, transition cutting district 2 and edge cutting district 3, the radius in center cutting district 1, the ring width in transition cutting district 2 and the ring width in edge cutting district 3 equal, the cutting off piece is weighed after drying and is cut off the quality of piece and is recorded as m4；
(III) cleaning the cut blocks with a cleaning agent, drying the cleaned cut blocks, weighing the cut blocks again after drying, and recording the mass m of the cut blocks5And calculating to obtain the infiltration parameters of the detection pole piece.
The method is adopted to respectively carry out electrolyte infiltration tests on the positive pole piece and the negative pole piece, the electrolyte comprises lithium hexafluorophosphate, the cleaning agent is dimethyl carbonate, the infiltration flow of the detection battery is constant temperature standing for 2 hours at 45 ℃, and the test result is shown in figure 4:
in the negative electrode sheet, AStandard of merit1.53 g/g; a of the center cutting area 1Analysis of1.48 g/g; a of transition cutting area 2Analysis of1.5 g/g; a of the edge trimming area 3Analysis ofIt was 1.52 g/g.
In the positive electrode sheet, AStandard of merit0.79 g/g; a of the center cutting area 1Analysis of0.75 g/g; a of transition cutting area 2Analysis of0.77 g/g; a of the edge trimming area 3Analysis ofIt was 0.78 g/g.
Through the embodiment, the electrolyte wettability test is carried out through a quality difference method, the wettability of the pole piece to the electrolyte is determined by combining the quality of the non-volatile substances in the electrolyte, the electrolyte wettability conditions of different positions in the detected pole piece are obtained on the basis of the wetting parameters of the standard pole piece, the difference of the pole piece to the electrolyte wettability is analyzed, and the wetting performance of the pole piece to the electrolyte can be determined only by analyzing the test data of the standard pole piece. The invention can measure the batteries in different working states and has the characteristics of simple test method, low cost, accurate measurement result and the like.
The applicant declares that the above description is only a specific embodiment of the present invention, but the scope of the present invention is not limited thereto, and it should be understood by those skilled in the art that any changes or substitutions that can be easily conceived by those skilled in the art within the technical scope of the present invention are within the scope and disclosure of the present invention.
Claims (10)
1. The method for testing the wettability of the electrolyte is characterized by comprising the following steps of:
taking a standard pole piece and a detection battery prepared by adopting the standard pole piece, dripping electrolyte on the standard pole piece and drying, and respectively weighing the weight of the standard pole piece before dripping the electrolyte, the quality of the dried standard pole piece and the dripping amount of the electrolyte;
the method comprises the following steps of disassembling a working detection battery, disassembling a pole piece in the detection battery to be the detection pole piece, cutting the detection pole piece into at least two cutting blocks, airing and weighing the cutting blocks in sequence, cleaning and drying the cutting blocks in sequence after weighing, weighing the cutting blocks again after drying, and obtaining the infiltration parameters of the detection pole piece.
2. The testing method according to claim 1, characterized in that the testing method specifically comprises the following steps:
taking a standard pole piece and a detection battery prepared by adopting the standard pole piece, and weighing the standard pole piece to be m1The dropping quality of the standard pole piece is recorded as m2The electrolyte is dried to a stable quality, and the weight of the pole piece is weighed again and recorded as m3；
(II) disassembling the working detection battery, taking out the detection pole piece and cutting at least two cutting blocks, weighing the mass of the cutting blocks after the cutting blocks are dried and recording the mass as m4；
(III) cleaning the cut blocks with a cleaning agent, drying the cleaned cut blocks, weighing the cut blocks again after drying, and recording the mass m of the cut blocks5And calculating to obtain the infiltration parameters of the detection pole piece.
3. The test method according to claim 2, wherein in the step (I), the injection standard is 0.8-3 g/g.
4. The test method according to claim 2 or 3, wherein in the step (I), preferably, the pole piece is dripped with the electrolyte under a dry environment;
preferably, the humidity of the dry environment is < 10%.
5. The test method according to any one of claims 2 to 4, wherein in the step (II), the pole piece is divided into a central cutting area, a transition cutting area and an edge cutting area along the central direction edge, and the cutting block is respectively cut in the central cutting area, the transition cutting area and the edge cutting area;
preferably, the center cutting area, the transition cutting area and the edge cutting area are arranged in a concentric circle or a concentric matrix at the center of the pole piece;
preferably, the radius of the central cutting area, the loop width of the transition cutting area and the loop width of the edge cutting area are equal.
6. The test method according to any one of claims 2 to 5, wherein in the step (III), the infiltration parameters include unit mass electrolyte infiltration amount of a standard pole piece, unit mass electrolyte content of different positions of a detection pole piece, and unit mass electrolyte infiltration amount of different positions of the detection pole piece.
7. The test method according to claim 6, wherein the infiltration amount of the electrolyte per unit mass of the standard pole piece is recorded as AStandard of meritSaid A isStandard of merit＝m2/m1。
8. The test method according to claim 6 or 7, wherein the detection pole piece is subjected to wet electrolysis at different positionsThe content of the hydrolyzed solution is recorded as mAnalysis ofM is saidAnalysis of＝(m4-m5)*m2/(m3-m1)。
9. The test method according to any one of claims 6 to 8, wherein the unit mass electrolyte infiltration capacity of the detection pole piece at different positions is recorded as AAnalysis ofSaid A isAnalysis of＝mAnalysis of/m5。
10. Use of the electrolyte wetting test method according to any one of claims 1 to 9 for measuring electrolyte wetting in a lithium ion battery.
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| CN114397219A (en) * | 2022-01-25 | 2022-04-26 | 上海兰钧新能源科技有限公司 | Infiltration duration measuring and calculating method and device |
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| CN114397219A (en) * | 2022-01-25 | 2022-04-26 | 上海兰钧新能源科技有限公司 | Infiltration duration measuring and calculating method and device |
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Application publication date: 20210625 |