CN114858256A - Method and equipment for measuring weight of lithium battery electrolyte by using solution dilution - Google Patents
Method and equipment for measuring weight of lithium battery electrolyte by using solution dilution Download PDFInfo
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- CN114858256A CN114858256A CN202210520761.4A CN202210520761A CN114858256A CN 114858256 A CN114858256 A CN 114858256A CN 202210520761 A CN202210520761 A CN 202210520761A CN 114858256 A CN114858256 A CN 114858256A
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- 239000003792 electrolyte Substances 0.000 title claims abstract description 57
- 238000000034 method Methods 0.000 title claims abstract description 45
- 239000000243 solution Substances 0.000 title claims abstract description 33
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 title claims abstract description 20
- 238000010790 dilution Methods 0.000 title claims abstract description 20
- 239000012895 dilution Substances 0.000 title claims abstract description 20
- 229910052744 lithium Inorganic materials 0.000 title claims abstract description 20
- 239000012086 standard solution Substances 0.000 claims abstract description 86
- 238000005070 sampling Methods 0.000 claims abstract description 54
- 238000007654 immersion Methods 0.000 claims abstract description 52
- 239000007788 liquid Substances 0.000 claims abstract description 26
- 239000011259 mixed solution Substances 0.000 claims abstract description 23
- 150000002500 ions Chemical class 0.000 claims abstract description 22
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 claims abstract description 15
- 229910001416 lithium ion Inorganic materials 0.000 claims abstract description 15
- 239000002904 solvent Substances 0.000 claims abstract description 14
- 238000006243 chemical reaction Methods 0.000 claims abstract description 8
- 239000008151 electrolyte solution Substances 0.000 claims abstract description 4
- 230000007246 mechanism Effects 0.000 claims description 30
- 238000002156 mixing Methods 0.000 claims description 26
- 238000007789 sealing Methods 0.000 claims description 23
- 229910001415 sodium ion Inorganic materials 0.000 claims description 14
- 238000003756 stirring Methods 0.000 claims description 12
- 239000000523 sample Substances 0.000 claims description 8
- 230000005284 excitation Effects 0.000 claims description 6
- 230000035939 shock Effects 0.000 claims description 6
- IEJIGPNLZYLLBP-UHFFFAOYSA-N dimethyl carbonate Chemical compound COC(=O)OC IEJIGPNLZYLLBP-UHFFFAOYSA-N 0.000 claims description 5
- 238000002354 inductively-coupled plasma atomic emission spectroscopy Methods 0.000 claims description 5
- 238000005259 measurement Methods 0.000 claims description 5
- 239000013543 active substance Substances 0.000 claims description 4
- 238000004364 calculation method Methods 0.000 claims description 4
- YLKTWKVVQDCJFL-UHFFFAOYSA-N sodium;bis(trifluoromethylsulfonyl)azanide Chemical compound [Na+].FC(F)(F)S(=O)(=O)[N-]S(=O)(=O)C(F)(F)F YLKTWKVVQDCJFL-UHFFFAOYSA-N 0.000 claims description 4
- KMTRUDSVKNLOMY-UHFFFAOYSA-N Ethylene carbonate Chemical compound O=C1OCCO1 KMTRUDSVKNLOMY-UHFFFAOYSA-N 0.000 claims description 3
- 238000004090 dissolution Methods 0.000 claims description 3
- JBTWLSYIZRCDFO-UHFFFAOYSA-N ethyl methyl carbonate Chemical compound CCOC(=O)OC JBTWLSYIZRCDFO-UHFFFAOYSA-N 0.000 claims description 3
- 239000012488 sample solution Substances 0.000 claims description 3
- 230000000694 effects Effects 0.000 claims 5
- 230000008859 change Effects 0.000 abstract description 4
- 230000000087 stabilizing effect Effects 0.000 abstract 1
- 238000002347 injection Methods 0.000 description 12
- 239000007924 injection Substances 0.000 description 12
- 230000008569 process Effects 0.000 description 8
- 238000012360 testing method Methods 0.000 description 8
- FKNQFGJONOIPTF-UHFFFAOYSA-N Sodium cation Chemical compound [Na+] FKNQFGJONOIPTF-UHFFFAOYSA-N 0.000 description 5
- 238000004519 manufacturing process Methods 0.000 description 4
- 238000012546 transfer Methods 0.000 description 4
- 238000004458 analytical method Methods 0.000 description 3
- 238000001035 drying Methods 0.000 description 2
- 230000014759 maintenance of location Effects 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 238000000691 measurement method Methods 0.000 description 2
- 239000003921 oil Substances 0.000 description 2
- 238000005303 weighing Methods 0.000 description 2
- QXZNUMVOKMLCEX-UHFFFAOYSA-N [Na].FC(F)(F)S(=O)(=O)NS(=O)(=O)C(F)(F)F Chemical compound [Na].FC(F)(F)S(=O)(=O)NS(=O)(=O)C(F)(F)F QXZNUMVOKMLCEX-UHFFFAOYSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 239000011149 active material Substances 0.000 description 1
- 230000006978 adaptation Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- -1 dimethyl carbonate Chemical compound 0.000 description 1
- 238000006073 displacement reaction Methods 0.000 description 1
- 238000002224 dissection Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 238000004146 energy storage Methods 0.000 description 1
- 239000000446 fuel Substances 0.000 description 1
- 239000004519 grease Substances 0.000 description 1
- 230000020169 heat generation Effects 0.000 description 1
- 159000000002 lithium salts Chemical group 0.000 description 1
- 230000001050 lubricating effect Effects 0.000 description 1
- 239000010687 lubricating oil Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012858 packaging process Methods 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 238000002791 soaking Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
- 239000013585 weight reducing agent Substances 0.000 description 1
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01G—WEIGHING
- G01G17/00—Apparatus for or methods of weighing material of special form or property
- G01G17/04—Apparatus for or methods of weighing material of special form or property for weighing fluids, e.g. gases, pastes
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/30—Staining; Impregnating ; Fixation; Dehydration; Multistep processes for preparing samples of tissue, cell or nucleic acid material and the like for analysis
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/62—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
- G01N21/71—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light thermally excited
- G01N21/73—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light thermally excited using plasma burners or torches
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P70/00—Climate change mitigation technologies in the production process for final industrial or consumer products
- Y02P70/50—Manufacturing or production processes characterised by the final manufactured product
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- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- General Physics & Mathematics (AREA)
- Pathology (AREA)
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- Immunology (AREA)
- Engineering & Computer Science (AREA)
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Abstract
The invention discloses a method for measuring the weight of lithium battery electrolyte by using solution dilution, which comprises the steps of preparing a standard solution, stabilizing each component of a lithium ion battery by the standard solution, ensuring that no chemical reaction occurs between the standard solution and the lithium ion battery, ensuring that solute does not exist in the battery to be measured, enabling a solvent and an electrolyte solution to be mutually soluble, placing the dissected battery into an immersion container, sampling mixed liquid in the battery at certain intervals, measuring the concentration of a standard ion in the mixed solution, calculating the mass of the electrolyte in a battery pack according to the diluted concentration of the standard ion in the standard solution when the concentration of the solute between the electrolyte and the standard solution is balanced, and accurately calculating the weight of the electrolyte in the original battery according to the relative change of the diluted concentration of the solute in the standard solution in the component.
Description
Technical Field
The invention belongs to the field of lithium ion batteries, and particularly relates to a method and equipment for measuring the weight of lithium battery electrolyte by using solution dilution.
Background
With the continuous increase of market demand, the application of the lithium ion battery in the fields of 3C and power energy storage is more and more extensive. In recent years, with the promotion of forbidden selling schedules of fuel vehicles in various countries, the new energy vehicles have more and more stable status, and lithium ion batteries are more and more popular in the market as core power sources of electric vehicles. The lithium ion battery relates to the selection and matching of materials such as an anode, electrolyte, a cathode, a diaphragm and the like, and the selection of pole piece design parameters and the like in the manufacturing process; the working process of the battery relates to the processes of chemical reaction, mass transfer, electric conduction, heat generation and the like. Thus, lithium ion batteries are a very complex system. The method also has important significance for analyzing various process parameters of the lithium ion battery.
The electrolyte injection amount in the battery is an important parameter of the lithium ion battery, and the content of the electrolyte can affect the electrical performance and the safety performance of the battery. There is no disclosure of how to accurately measure the weight of electrolyte in a battery with an unknown electrolyte injection amount.
The following methods are generally adopted in the industry to test the liquid retention capacity of the battery:
1) in the manufacturing process of the battery, after the battery is fully dried, the total weight V0 of the primary battery is measured before liquid injection, and then liquid injection is carried out; after the liquid injection, the total weight of the battery V1 was measured, and the battery was subjected to the standing process and the formation process, and the final total weight of the packaged battery V2 was measured. Wherein V1-V0 are actual liquid injection amount of the battery (electrolyte error from liquid injection process is eliminated), and V2-V0 are actual liquid retention amount in the battery (electrolyte error from post-liquid injection process to packaging process is eliminated). The method is simple and effective, and is suitable for mass production; however, the method is limited to the control of the electrolyte weight in the battery manufacturing process, and if a finished battery with unknown liquid injection amount is taken during product analysis, the electrolyte weight cannot be measured due to the fact that V0 is unknown.
2) Baking and weight reduction; if a finished battery with unknown liquid injection amount is taken when product analysis is carried out, the general analysis method comprises the following steps: weighing the battery to obtain the total weight V0 of the battery, dissecting the battery in a dry environment, decomposing the battery into components such as a positive plate, a negative plate, a diaphragm, a shell and the like, volatilizing the electrolyte solvent of the components in an environment of 80-100 ℃, and completely drying. After the liquid is completely dried, drying each component and then weighing, wherein the sum of the weights is V1; the weight of V0-V1 is defined as the approximate value of the weight of the electrolyte. According to the method, the pole piece is subjected to powder falling in the process of battery dissection, lithium salt residues still exist after the electrolyte solvent is dried, water absorption is possibly caused when the pole piece is weighed after being dried, the operation time is long, and uncontrollable factors are more, so that the method is low in precision and only can be used as a rough reference.
The two measurement methods are difficult to measure the residual electrolyte of the battery with unknown liquid injection amount or cannot accurately measure the residual electrolyte, so that a method for accurately measuring the residual electrolyte of the battery with unknown liquid injection amount is needed.
Disclosure of Invention
The purpose of the invention is as follows: in order to overcome the defects in the prior art, the invention provides a method and equipment for measuring the weight of lithium battery electrolyte by using solution dilution
The technical scheme is as follows: in order to achieve the purpose, the technical scheme of the invention is as follows:
a method for measuring the weight of a lithium battery electrolyte using solution dilution, comprising:
the method comprises the following steps: preparing a standard solution, wherein the concentration of the standard solution is C standard, the mass of the standard solution is m standard, the volume of the standard solution is V standard, the density of the standard solution is rho standard, the standard solution is stable to each component of the lithium ion battery, no chemical reaction occurs between the standard solution and the lithium ion battery, a solute does not exist in the battery to be measured, and a solvent and an electrolyte solution are mutually soluble;
step two: dissecting the battery shell in a dry environment to expose part of the battery electrolyte;
step three: placing the dissected battery into an immersion container, adding standard solution into the immersion container, and enabling the standard solution to completely immerse the battery;
step four: sealing the immersion container, and carrying out mutual dissolution reaction in a dry environment;
step five: sampling the mixed liquid in the battery at regular intervals, wherein the sampling mass is ma, the volume is Va, measuring the concentration of the calibration ions in the mixed solution by using an ICP-OES method, and defining the concentration of the calibration ions in the measured mixed solution as Ca;
step six: when the solute concentration between the electrolyte and the standard solution reaches the equilibrium, the concentration of the standard ions in the mixed solution is Cn.a, and then the mass of the electrolyte in the battery pack is calculated according to the diluted concentration of the standard ions in the standard solution.
Furthermore, the solute of the standard solution is 1mol/L NaTFSI, the calibration ion is sodium ion, and the solvent is any one of dimethyl carbonate, ethyl methyl carbonate and ethylene carbonate.
Further, the standard solution data and the measurement data are substituted into the calculation formula:
in the formula: and C, marking: the concentration of the standard solution; m marks: quality of standard solution; and V mark: standard solution volume; rho mark: standard solution density; cn.a: sampling concentration of the standard solution for the nth time; a, mn.a: sampling quality of the standard solution for the nth time; a: sample volume n of standard solution.
Furthermore, when the battery is immersed in the solution, active substances in the electrolyte are mutually soluble with the solute, and the mixed solution in the immersion container is vibrated or stirred, so that the solute and the solvent of the mixed solution are dynamically and uniformly mixed.
Furthermore, when sampling, a plurality of sampling points are sampled at different positions and different depths in the immersion container, and the sampled sample solution is fully and uniformly mixed and then is subjected to calibration ion concentration measurement.
Further, the device for implementing the method for measuring the weight of the lithium battery electrolyte by using solution dilution comprises an immersion container, a disturbance mechanism, a sampling pipe group and a mixing container, wherein the disturbance mechanism is arranged in the immersion container, the disturbance mechanism disturbs the standard solution in the immersion container, the top wall of the immersion container comprises a plurality of sampling points, the sampling pipe group is arranged corresponding to the sampling points, the sampling end of the sampling pipe group extends into the inner cavity of the immersion container, and the liquid outlet end of the sampling pipe group is communicated with the mixing container.
Furthermore, a plurality of sampling points are communicated with one another to form a movable groove of an annular structure, a sliding block is movably arranged in the movable groove, and the sliding block is adjusted relative to the position of the immersion container through the movable groove; the top wall of the immersion container is divided into an outer ring wall and an inner ring wall through a movable groove, a plurality of groups of supporting frames are arranged on the inner ring wall along the edge contour, the inner ring wall is relatively and fixedly connected to the outer ring wall through the plurality of groups of supporting frames, and the sliding blocks are annularly and slidably arranged in the movable groove.
Furthermore, a sealing strip is arranged in the movable groove in a relatively sliding and sealing manner, and two ends of the sealing strip are abutted against or connected to the sliding block; the sliding block enables the sealing strip to move along with the movable groove in a sliding state.
Furthermore, a mixing mechanism is arranged in the mixing container, the mixing mechanism comprises a stirring rod, two ends of the stirring rod are rotatably arranged on the wall body of the mixing container, an axial flow fan is coaxially arranged at the top end of the stirring rod, and the axial flow fan is arranged right corresponding to the liquid inlet of the mixing container; the solution entering the mixing vessel drives the stirring rod to rotate.
Further, disturbance mechanism includes movable base, resets and shakes the mechanism with swashing, movable base slides and sets up bottom in the inner chamber of immersion container, just movable base through reset an elastic connection in immersion container's lateral wall, be provided with shakes the mechanism with swashing between movable base and immersion container's the lateral wall, shake the reciprocal standard solution that vibrates of mechanism drive movable base with swashing.
Has the advantages that: the invention adopts a standard solution which is stable for each component of the lithium battery and has no solute existing in the battery to be calibrated, the standard solution is used for soaking chemical substances in the battery integrally, and a certain amount of mixed solution is taken out for testing the components after the solute and the solvent of the standard solution and the solution of the electrolyte in the battery reach concentration balance. According to the relative change of the concentration of the diluted solute in the standard solution in the components, the weight of the electrolyte in the original battery can be accurately calculated.
Drawings
FIG. 1 is a schematic overall flow chart of the measurement method of the present invention;
FIG. 2 is a perspective view of the overall structure of the test apparatus of the present invention;
FIG. 3 is a schematic half-section view of the overall structure of the test apparatus of the present invention;
FIG. 4 is a schematic diagram of the internal structure of the test apparatus of the present invention;
FIG. 5 is an enlarged view of the structure of part A of the test apparatus of the present invention;
fig. 6 is an enlarged schematic view of the structure of part B of the test apparatus of the present invention.
Detailed Description
The present invention will be further described with reference to the accompanying drawings.
As shown in fig. 1, a method for measuring the weight of an electrolyte of a lithium battery by using solution dilution comprises the following steps:
the method comprises the following steps: preparing a standard solution, wherein the concentration of the standard solution is C standard, the mass of the standard solution is m standard, the volume of the standard solution is V standard, the density of the standard solution is rho standard, the standard solution is stable to each component of the lithium ion battery, no chemical reaction occurs between the standard solution and the lithium ion battery, a solute does not exist in the battery to be measured, and a solvent and an electrolyte solution are mutually soluble;
the solute of the standard solution is 1mol/L NaTFSI (sodium bis (trifluoromethylsulfonyl) imide), the calibration ion is sodium ion, the calibration ion is ion detected during concentration measurement, and the solvent comprises any one of dimethyl carbonate, ethyl methyl carbonate and ethylene carbonate, but is not limited to the above.
Step two: dissecting the battery shell in a dry environment to expose part of the battery electrolyte; under the condition that the dew point is-30 ℃, an opening of a battery shell is dissected, so that the interior of the battery core is leaked out;
step three: placing the dissected battery into an immersion container, adding standard solution into the immersion container, and enabling the standard solution to completely immerse the battery;
step four: sealing the immersion container, and carrying out mutual dissolution reaction in a dry environment;
step five: sampling the mixed liquid in the battery at regular intervals, wherein the sampling mass is ma, the volume is Va, measuring the concentration of the calibration ions in the mixed solution by using an ICP-OES method, and defining the concentration of the calibration ions in the measured mixed solution as Ca;
step six: when the solute concentration between the electrolyte and the standard solution reaches the equilibrium, the concentration of the standard ions in the mixed solution is Cn.a, and then the mass of the electrolyte in the battery pack is calculated according to the diluted concentration of the standard ions in the standard solution.
Substituting the standard solution data and the measured data into a calculation formula:
in the formula: and C, marking: the concentration of the standard solution; m marks: quality of standard solution; and V mark: standard solution volume; rho mark: standard solution density; cn.a: sampling concentration of the standard solution for the nth time; a, mn.a: sampling quality of the standard solution for the nth time; a: sample volume n of standard solution. The calculation method considers the changes of the system volume and the density of the mixed solution after the standard solution is mixed with the electrolyte.
In a dry environment, after the opening of the battery shell is dissected, the whole battery shell is integrally placed in a container which is slightly larger than the size of the battery. Preparing a standard solution, wherein the concentration is C standard, the mass is m standard, the volume is V standard, and the density is rho standard; dosed into the container and the standard solution completely submerged the cell active. And then sealing the container and standing at normal temperature in a dry environment. The mixed liquid in the cell was sampled at regular intervals (a hours) with a sampling mass ma and a volume Va. And testing the concentration of sodium ions in the standard solution by using ICP-OES, defining the concentration of the sodium ions in the tested mixed solution as Ca, and when the concentration change of the sodium ions sampled twice is smaller than a set value, considering that the solute concentration between the electrolyte and the standard solution reaches equilibrium. At the moment, the concentration ratio Cn.a of sodium ions in the diluted mixed solution is tested, and the mass of the electrolyte in the original battery can be accurately converted.
An experimental sample: the prepared standard solution has the solute of NaTFSI and the solvent of DMC, namely dimethyl carbonate, and the concentration of C is 1 mol/L. The mass of the standard solution added into the container is that the m is 300 g; volume, vtag 0.267L, density, ρ ag 1.12g/cm 3; the standard solution completely immerses the battery active. Then sealing the container and standing at normal temperature under the environment with dew point of-30 ℃. Sampling the mixed liquid in the battery at regular intervals (1 hour), wherein the sampling mass is ma which is 2.38 g; the volume was Va ═ 2 mL. The sodium ion concentration in the standard solution was measured by ICP-OES, and the sodium ion concentration in the mixed solution was defined as Ca. When the change in the sodium ion concentration of the 4 th and 5 th samples was measured to be less than 15ppm, we considered that the concentration of the electrolyte in the cell was in equilibrium with the standard solution added. The concentration ratio c5.a of sodium ions in the diluted mixed solution was measured to be 0.66mol/L, and the mass of the electrolyte in the original battery was accurately calculated to be 135 g.
When the battery is immersed in the solution, active substances in the electrolyte and the solute are mutually dissolved, and meanwhile, the mixed solution in the immersion container is vibrated or stirred, so that the solute and the solvent of the mixed solution are dynamically and uniformly mixed.
When sampling, a plurality of sampling points are sampled at different positions and different depths in the immersion container, and the sampled sample solution is fully and uniformly mixed and then is subjected to calibration ion concentration measurement.
As shown in fig. 2 to 6, an apparatus for implementing a method for measuring weight of lithium battery electrolyte by using solution dilution includes an immersion container 1, a disturbing mechanism 2, a sampling tube group 3 and a mixing container 4, the disturbing mechanism 2 is disposed in the immersion container 1, the disturbing mechanism 2 disturbs a standard solution in the immersion container, and since sodium ions are mutually soluble with active substances in the electrolyte near a battery pack 10, sodium ions are unevenly distributed in the mixed solution near the battery pack and in other areas, if the apparatus is only in a standing state, the apparatus may cause disadvantages of low mutual solubility efficiency and long period, and disturbs the immersed solution, so that sodium ions in the immersed solution are evenly distributed, and mutual solubility efficiency is improved. The top wall of the immersion container 1 comprises a plurality of sampling points, a sampling pipe group 3 is arranged corresponding to the sampling points, the sampling end of the sampling pipe group 3 extends into the inner cavity of the immersion container 1, and the liquid outlet end of the sampling pipe group 3 is communicated with the mixing container 4. By sampling and mixing the solution in the immersion container at multiple points, the uniformity and representativeness of the sampled solution can be improved.
The sampling points are mutually communicated and form a movable groove 5 with an annular structure, a sliding block 6 is movably adjusted in the movable groove 5, and the sliding block 6 is adjusted relative to the position of the immersion container 1 through the movable groove 5; the top wall of the immersion container 1 is divided into an outer ring wall 11 and an inner ring wall 12 through a movable groove 5, the inner ring wall 12 is provided with a plurality of groups of supporting frames 13 along the edge outline, the inner ring wall 12 is relatively fixedly connected to the outer ring wall 11 through the plurality of groups of supporting frames 13, and the sliding block 6 is annularly and slidably arranged in the movable groove. Support frame 13 is U type plate structure, the both ends of support frame 13 are connected respectively in inner circle wall 12 and outer lane wall 11 to make the inner circle wall relatively be fixed in the outer lane wall, form annular structure's movable groove, and the U type space of support frame 13 downwardly extending is used for making the sampling end pass through smoothly.
As shown in fig. 4 and 5, a sealing strip 7 is arranged in the movable groove 5 in a relatively sliding and sealing manner, and two ends of the sealing strip 7 are abutted against or connected to the sliding block 6; the sliding block 6 enables the sealing strip 7 to move along in the movable groove in a sliding state. The sealing strip 7 is made of flexible materials with an I-shaped section, such as rubber strips, and two ends of the sealing strip 7 are abutted against or connected to the sliding block 6; the slider 6 enables the sealing strip 7 to follow up in a sliding state, and the movable groove can be sealed through the sealing strip 7, so that the immersion container 1 is sealed, and the external environment pollution or the immersion solution interference is avoided.
Lubricating oil or lubricating grease is coated between the sealing strip 7 and the movable groove 5, so that the sealing strip can move smoothly, and an oil film can be formed at the sliding position to seal the oil.
As shown in fig. 3 and fig. 6, a mixing mechanism is arranged in the mixing container 2, the mixing mechanism includes a stirring rod 21, two ends of the stirring rod 21 are rotatably arranged on a wall body of the mixing container, an axial flow fan 22 is coaxially arranged at the top end of the stirring rod 21, and the axial flow fan 22 is arranged corresponding to a liquid inlet of the mixing container 2; the solution entering the mixing container drives the stirring rod to rotate, so that the sampling solution is further mixed without an additional driving mechanism.
As shown in fig. 3 and fig. 4, the disturbing mechanism includes a movable base 23, a reset member 24 and a shock excitation mechanism 25, the movable base 23 is slidably disposed at the bottom of the inner cavity of the immersion container 1, the bottom of the immersion container is provided with a plurality of groups of pulley blocks 27 corresponding to the movable base 23, on one hand, the movable base is supported, on the other hand, the movable base is used for promoting the smoothness of displacement, the movable base 23 is provided with a clamping mechanism 26 for clamping the battery pack, the movable base 23 is elastically connected to the side wall of the immersion container through the reset member, the shock excitation mechanism 25 is disposed between the movable base 23 and the side wall of the immersion container 1, and the shock excitation mechanism drives the movable base 23 to oscillate the standard solution in a reciprocating manner. The battery package is vibrated for the immersion container through disturbance mechanism, can make the abundant active material with in the battery package of immersion solution carry out mutually soluble, accelerates the dilution of sodion and promotes sodion distribution uniformity.
The above description is only of the preferred embodiments of the present invention, and it should be noted that: it will be apparent to those skilled in the art that various modifications and adaptations can be made without departing from the principles of the invention and these are intended to be within the scope of the invention.
Claims (10)
1. A method for measuring the weight of lithium battery electrolyte by using solution dilution is characterized in that: the method comprises the following steps:
the method comprises the following steps: preparing a standard solution, wherein the concentration of the standard solution is C standard, the mass of the standard solution is m standard, the volume of the standard solution is V standard, the density of the standard solution is rho standard, the standard solution is stable to each component of the lithium ion battery, no chemical reaction occurs between the standard solution and the lithium ion battery, a solute does not exist in the battery to be measured, and a solvent and an electrolyte solution are mutually soluble;
step two: dissecting the battery shell in a dry environment to expose part of the battery electrolyte;
step three: placing the dissected battery into an immersion container, adding standard solution into the immersion container, and enabling the standard solution to completely immerse the battery;
step four: sealing the immersion container, and carrying out mutual dissolution reaction in a dry environment;
step five: sampling the mixed liquid in the battery at regular intervals, wherein the sampling mass is ma, the volume is Va, measuring the concentration of the calibration ions in the mixed solution by using an ICP-OES method, and defining the concentration of the calibration ions in the measured mixed solution as Ca;
step six: when the solute concentration between the electrolyte and the standard solution reaches the equilibrium, the concentration of the standard ions in the mixed solution is Cn.a, and then the mass of the electrolyte in the battery pack is calculated according to the diluted concentration of the standard ions in the standard solution.
2. The method of claim 1, wherein the weight of the electrolyte of the lithium battery is measured by dilution with a solution, the method comprising: the solute of the standard solution is 1mol/L NaTFSI, the calibration ions are sodium ions, and the solvent is any one of dimethyl carbonate, ethyl methyl carbonate and ethylene carbonate.
3. The method of claim 1, wherein the weight of the electrolyte of the lithium battery is measured by dilution with a solution, the method comprising: substituting the standard solution data and the measured data into a calculation formula:
in the formula: and C, marking: the concentration of the standard solution; m marks: quality of standard solution; and V mark: standard solution volume; rho mark: standard solution density; cn.a: sampling concentration of the standard solution for the nth time; a, mn.a: sampling quality of the standard solution for the nth time; a: sample volume n of standard solution.
4. The method of claim 1, wherein the weight of the electrolyte of the lithium battery is measured by dilution with a solution, the method comprising: when the battery is immersed in the solution, active substances in the electrolyte and the solute are mutually dissolved, and meanwhile, the mixed solution in the immersion container is vibrated or stirred, so that the solute and the solvent of the mixed solution are dynamically and uniformly mixed.
5. The method of claim 1, wherein the weight of the electrolyte of the lithium battery is measured by dilution with a solution, the method comprising: when sampling, a plurality of sampling points are sampled at different positions and different depths in the immersion container, and the sampled sample solution is fully and uniformly mixed and then is subjected to calibration ion concentration measurement.
6. An apparatus for performing a method for measuring the weight of an electrolyte for a lithium battery using dilution with a solution according to claim 1, wherein: including immersion container (1), disturbance mechanism (2), sample nest of tubes (3) and mixing container (4), be provided with disturbance mechanism (2) in immersion container (1), the standard solution in disturbance mechanism (2) disturbance immersion container, include a plurality of sampling points on the roof of immersion container (1), be provided with sample nest of tubes (3) corresponding to the sampling point, the sampling end of sample nest of tubes (3) stretches into to the inner chamber of immersion container (1) in, the play liquid end of sample nest of tubes (3) communicates in mixing container (4) setting.
7. The apparatus of claim 6 for a method of measuring weight of electrolyte of lithium battery using dilution of solution, wherein: the sampling points are mutually communicated and form a movable groove (5) of an annular structure, a sliding block (6) is movably adjusted in the movable groove (5), and the sliding block (6) is adjusted in position relative to the immersion container (1) through the movable groove (5); the top wall of the immersion container (1) is divided into an outer ring wall (11) and an inner ring wall (12) through a movable groove (5), the inner ring wall (12) is provided with a plurality of groups of supporting frames (13) along the edge outline, the inner ring wall (12) is relatively fixedly connected to the outer ring wall (11) through the plurality of groups of supporting frames (13), and the sliding block (6) is arranged in the movable groove in an annular sliding manner.
8. The apparatus of claim 7 for a method of measuring weight of electrolyte of lithium battery using dilution of solution, wherein: a sealing strip (7) is arranged in the movable groove (5) in a relatively sliding and sealing manner, and two ends of the sealing strip (7) are abutted against or connected to the sliding block (6); the sliding block (6) enables the sealing strip (7) to move along with the movable groove in a sliding state.
9. The apparatus of claim 6 for a method of measuring weight of electrolyte of lithium battery using dilution of solution, wherein: a mixing mechanism is arranged in the mixing container (2), the mixing mechanism comprises a stirring rod (21), two ends of the stirring rod (21) are rotatably arranged on the wall body of the mixing container, an axial flow fan (22) is coaxially arranged at the top end of the stirring rod (21), and the axial flow fan (22) is arranged right corresponding to the liquid inlet of the mixing container (2); the solution entering the mixing vessel drives the stirring rod to rotate.
10. The apparatus of claim 6 for a method of measuring weight of electrolyte of lithium battery using dilution of solution, wherein: disturbance mechanism is including activity base (23), piece (24) and shock excitation mechanism (25) reset, activity base (23) slide and set up bottom in the inner chamber of immersion container (1), just activity base (23) through resetting a piece elastic connection in immersion container's lateral wall, be provided with shock excitation mechanism (25) between the lateral wall of activity base (23) and immersion container (1), shock excitation mechanism drive activity base (23) standard solution that vibrates reciprocally.
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