CN112748103A - Method for measuring content of liquid electrolyte in battery - Google Patents
Method for measuring content of liquid electrolyte in battery Download PDFInfo
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- CN112748103A CN112748103A CN202011537341.4A CN202011537341A CN112748103A CN 112748103 A CN112748103 A CN 112748103A CN 202011537341 A CN202011537341 A CN 202011537341A CN 112748103 A CN112748103 A CN 112748103A
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- 238000000034 method Methods 0.000 title claims abstract description 40
- 239000011244 liquid electrolyte Substances 0.000 title claims abstract description 15
- 239000012086 standard solution Substances 0.000 claims abstract description 86
- 239000003792 electrolyte Substances 0.000 claims abstract description 69
- 239000011259 mixed solution Substances 0.000 claims abstract description 54
- 150000002500 ions Chemical class 0.000 claims abstract description 50
- 239000007788 liquid Substances 0.000 claims abstract description 19
- 239000003960 organic solvent Substances 0.000 claims description 21
- 229910001414 potassium ion Inorganic materials 0.000 claims description 13
- 229910001415 sodium ion Inorganic materials 0.000 claims description 13
- FKNQFGJONOIPTF-UHFFFAOYSA-N Sodium cation Chemical compound [Na+] FKNQFGJONOIPTF-UHFFFAOYSA-N 0.000 claims description 10
- -1 cesium ions Chemical class 0.000 claims description 7
- VCCATSJUUVERFU-UHFFFAOYSA-N sodium bis(fluorosulfonyl)azanide Chemical compound FS(=O)(=O)N([Na])S(F)(=O)=O VCCATSJUUVERFU-UHFFFAOYSA-N 0.000 claims description 7
- KMTRUDSVKNLOMY-UHFFFAOYSA-N Ethylene carbonate Chemical compound O=C1OCCO1 KMTRUDSVKNLOMY-UHFFFAOYSA-N 0.000 claims description 6
- JBTWLSYIZRCDFO-UHFFFAOYSA-N ethyl methyl carbonate Chemical compound CCOC(=O)OC JBTWLSYIZRCDFO-UHFFFAOYSA-N 0.000 claims description 6
- 150000003949 imides Chemical class 0.000 claims description 6
- 239000000203 mixture Substances 0.000 claims description 6
- RUOJZAUFBMNUDX-UHFFFAOYSA-N propylene carbonate Chemical compound CC1COC(=O)O1 RUOJZAUFBMNUDX-UHFFFAOYSA-N 0.000 claims description 6
- HZNVUJQVZSTENZ-UHFFFAOYSA-N 2,3-dichloro-5,6-dicyano-1,4-benzoquinone Chemical compound ClC1=C(Cl)C(=O)C(C#N)=C(C#N)C1=O HZNVUJQVZSTENZ-UHFFFAOYSA-N 0.000 claims description 5
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical group [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 claims description 5
- IEJIGPNLZYLLBP-UHFFFAOYSA-N dimethyl carbonate Chemical compound COC(=O)OC IEJIGPNLZYLLBP-UHFFFAOYSA-N 0.000 claims description 5
- 229910001416 lithium ion Inorganic materials 0.000 claims description 5
- MHEBVKPOSBNNAC-UHFFFAOYSA-N potassium;bis(fluorosulfonyl)azanide Chemical compound [K+].FS(=O)(=O)[N-]S(F)(=O)=O MHEBVKPOSBNNAC-UHFFFAOYSA-N 0.000 claims description 5
- OIFBSDVPJOWBCH-UHFFFAOYSA-N Diethyl carbonate Chemical compound CCOC(=O)OCC OIFBSDVPJOWBCH-UHFFFAOYSA-N 0.000 claims description 4
- CPELXLSAUQHCOX-UHFFFAOYSA-M Bromide Chemical compound [Br-] CPELXLSAUQHCOX-UHFFFAOYSA-M 0.000 claims description 3
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 claims description 3
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 claims description 3
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 claims description 3
- VMHLLURERBWHNL-UHFFFAOYSA-M Sodium acetate Chemical compound [Na+].CC([O-])=O VMHLLURERBWHNL-UHFFFAOYSA-M 0.000 claims description 3
- 229910052792 caesium Inorganic materials 0.000 claims description 3
- 229910052700 potassium Inorganic materials 0.000 claims description 3
- 239000011591 potassium Substances 0.000 claims description 3
- 229910001419 rubidium ion Inorganic materials 0.000 claims description 3
- 229910052708 sodium Inorganic materials 0.000 claims description 3
- 239000011734 sodium Substances 0.000 claims description 3
- 235000017281 sodium acetate Nutrition 0.000 claims description 3
- 239000001632 sodium acetate Substances 0.000 claims description 3
- 150000001733 carboxylic acid esters Chemical class 0.000 claims 1
- 238000012360 testing method Methods 0.000 description 13
- 239000000243 solution Substances 0.000 description 12
- NPYPAHLBTDXSSS-UHFFFAOYSA-N Potassium ion Chemical compound [K+] NPYPAHLBTDXSSS-UHFFFAOYSA-N 0.000 description 9
- 238000005070 sampling Methods 0.000 description 7
- 238000002354 inductively-coupled plasma atomic emission spectroscopy Methods 0.000 description 6
- 239000012470 diluted sample Substances 0.000 description 5
- 238000001514 detection method Methods 0.000 description 4
- 238000005259 measurement Methods 0.000 description 3
- 239000002904 solvent Substances 0.000 description 3
- 229910021201 NaFSI Inorganic materials 0.000 description 2
- 150000007942 carboxylates Chemical class 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 230000029087 digestion Effects 0.000 description 2
- 238000004146 energy storage Methods 0.000 description 2
- 238000006467 substitution reaction Methods 0.000 description 2
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 1
- 229910001413 alkali metal ion Inorganic materials 0.000 description 1
- 150000001450 anions Chemical class 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 125000005587 carbonate group Chemical group 0.000 description 1
- 238000002485 combustion reaction Methods 0.000 description 1
- XMBWDFGMSWQBCA-UHFFFAOYSA-N hydrogen iodide Chemical compound I XMBWDFGMSWQBCA-UHFFFAOYSA-N 0.000 description 1
- 229910017604 nitric acid Inorganic materials 0.000 description 1
- 230000010412 perfusion Effects 0.000 description 1
- 239000012488 sample solution Substances 0.000 description 1
- 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 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
Images
Classifications
-
- 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
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
-
- 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
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
Abstract
A method for determining the content of liquid electrolyte in a battery is provided, which comprises the following steps: preparing a standard solution with predetermined ions, wherein the electrolyte does not contain the predetermined ions; preparing a battery needing to measure the content of the electrolyte; adding a preset amount of standard solution into the battery, and mixing the standard solution with the electrolyte in the battery to form a mixed solution; determining the concentration of the preset ions in the mixed solution and the standard solution of unit mass; and determining the electrolyte mass in the battery. The determination method provided by the invention is simple to operate and easy to implement, and the content accuracy of the detected battery electrolyte is high, the error is small, and the method can be used for distinguishing a solid-liquid battery from a liquid battery and has high feasibility.
Description
Technical Field
The invention belongs to the technical field of battery correlation, and particularly relates to a method for measuring the content of liquid electrolyte in a battery.
Background
In recent years, with the development of electric vehicles and the development of the demand for grid energy storage and small-sized energy storage, it is necessary to develop a battery that can be used in a wide temperature range and has high safety, high energy density, and high power density. According to different application scenes, the electrolyte perfusion amount in the single battery can be several grams or dozens of grams to several hundred grams, and because the electrolyte has potential safety hazards of easy leakage, easy volatilization, easy combustion and the like, how to conveniently and accurately detect the electrolyte content in the battery is an important link for ensuring the safety of a battery product.
However, there is no specific method for detecting the content of the electrolyte in the battery, so a feasible operation method for conveniently determining the content of the electrolyte in the battery is needed.
Disclosure of Invention
In order to solve the above problems in the prior art, the present invention provides a method for measuring the content of a liquid (e.g., a liquid electrolyte) in a battery, which is simple and easy to implement and can be used for measuring the content of the liquid such as the liquid electrolyte in various batteries.
According to an exemplary embodiment, a method of determining the content of a liquid electrolyte in a battery includes the steps of:
s1, preparing a standard solution with preset ions, wherein the electrolyte does not contain the preset ions;
s2: preparing a battery needing to measure the content of the liquid electrolyte;
s3: adding a preset amount of standard solution into the battery, and mixing the standard solution with the electrolyte in the battery to form a mixed solution;
s4: determining the concentration of the preset ions in the mixed solution and the standard solution of unit mass;
s5: determining an electrolyte mass in the battery, which is determined by the following equation:
wherein m is1M is the mass of the electrolyte2Is the mass of the predetermined amount of the standard solution, c1Is a predetermined ion concentration in the mixed liquid per unit mass, c2Is the predetermined ion concentration in the standard solution per unit mass.
In some examples, the predetermined ions contained in the standard solution may be sodium ions, potassium ions, rubidium ions, cesium ions, bromide ions, chloride ions, or iodide ions.
In some examples, the concentration of the predetermined ion in the standard solution is equal to or greater than 0.001mol/L, the upper limit of which is its solubility in the standard solution, and the concentration is preferably 0.05 to 1 mol/L.
In some examples, the standard solution may be prepared by dissolving one of sodium bis (trifluorosulfonyl) imide, sodium bis (fluorosulfonyl) imide, sodium acetate, potassium hexafluorophosphate, potassium bis (trifluorosulfonyl) imide, and potassium bis (fluorosulfonyl) imide in an organic solvent.
In some examples, the organic solvent is a carbonate and/or carboxylate organic solvent, such as any one or a mixture of two or more of Ethylene Carbonate (EC), Propylene Carbonate (PC), dimethyl carbonate (DMC), Ethyl Methyl Carbonate (EMC) diethyl carbonate (DEC), and carboxylate organic solvents (MF, MA, EA, MA, MP).
In some examples, in step S3, in order to ensure that the electrolyte and the standard solution are sufficiently mixed, the mixed solution may be accelerated to be mixed by using a mixing device such as a vibration instrument or a rotation instrument after the mixed solution is left standing for a certain period of time.
In some examples, in step S4, a unit mass of the mixed solution and a unit mass of the standard solution may be taken from the mixed solution and the standard solution, the mixed solution and the standard solution may be fixed to the same volume, the predetermined ion concentrations in the mixed solution and the standard solution after the fixed volume are measured, and the predetermined ion concentrations in the mixed solution and the standard solution may be determined according to the measured predetermined ion concentrations in the mixed solution and the standard solution after the fixed volume is determined.
In some examples, the battery is a lithium ion battery or a sodium ion battery.
In some examples, the battery is any one of a pouch battery, a square battery, and a cylindrical battery.
The invention has the following beneficial effects:
the method for measuring the content of the electrolyte is simple to operate and easy to implement, the result of the content of the electrolyte measured by the method is high in accuracy, and compared with the actual content, the error is small (the error is less than 5%).
Other features and advantages of the present invention will become apparent from the description of exemplary embodiments.
Drawings
Fig. 1 shows a flow chart of a method of determining the electrolyte content in a battery according to an exemplary embodiment of the present invention.
Detailed Description
The present invention is further illustrated by the following specific examples, which are provided by way of illustration only and are not to be construed as limiting the scope of the invention.
Fig. 1 shows a flowchart of a method for determining the content of a liquid electrolyte in a battery according to an exemplary embodiment of the present invention. As shown in fig. 1, the method 100 may begin with step S1 by preparing a standard solution having predetermined ions that may be selected based on the composition of the liquid battery electrolyte such that the predetermined ions are not present in the liquid battery electrolyte and, preferably, the predetermined ions do not react with the electrolyte. In one example, the predetermined ion may be selected from alkali metal ions. For example, for a lithium ion battery, the predetermined ions may be selected from sodium ions and potassium ions, and for a sodium ion battery, the predetermined ions may be selected from potassium ions, rubidium ions and cesium ions. In one example, the predetermined ion may also be selected from anions, such as a halide ion, such as bromide, chloride, or iodide.
To prepare a standard solution, in one embodiment, the salt compound of the predetermined ion and the solvent may be optionally mixed and stirred. The compound that can be used in the standard solution can be one or more selected from sodium bis (trifluorosulfonyl) imide, sodium bis (fluorosulfonyl) imide, sodium acetate, potassium hexafluorophosphate, potassium bis (trifluorosulfonyl) imide and potassium bis (fluorosulfonyl) imide, and the solvent that can be used in the standard solution can be an organic solvent, for example, the same organic solvent as that in the electrolyte of a lithium ion battery can be selected, so that the subsequent uniform mixing of the standard solution and the electrolyte can be promoted. In some examples, standard solutions can be prepared by dissolving the compounds in an organic solvent and mixing well.
In some examples, the concentration of the predetermined ion in the standard solution is equal to or greater than 0.001mol/L, with the upper limit being its solubility in the standard solution. It should be noted that, since the method for determining the electrolyte content does not need to know the concentration of the predetermined ion in the standard solution, the present invention is not particularly limited to the concentration of the predetermined ion in the standard solution, but in order to ensure the accuracy of the subsequent determination of the predetermined ion, the standard solution with the concentration of 0.05 to 1mol/L, and more preferably 0.1 to 0.5mol/L, may be preferably selected.
In step S2, a battery whose electrolyte content needs to be measured is prepared. This step and the sequence of step S1 may be performed simultaneously or sequentially, and the present invention is not particularly limited.
As described above, in some examples, the battery may be a lithium ion battery or a sodium ion battery. Specifically, the battery may be in the form of any one of a pouch battery, a square battery, and a cylindrical battery.
Next, in step S3, a predetermined amount is added to the battery(m2) The standard solution of (2) is mixed with the electrolyte in the battery to form a mixed solution. In one embodiment, the mass of the added standard solution may be determined according to the specifications of the liquid battery to ensure that the subsequent determination of the predetermined ion concentration is accurate. For example, for a liquid battery with a fill volume of several tens of grams, it is conceivable to add 5 to 50g of standard solution.
In some examples, in step S3, in order to ensure that the electrolyte and the standard solution are sufficiently mixed, the mixed solution may be accelerated to be mixed by using a vibration device such as a vibration instrument or a rotator after the mixed solution is left to stand for a certain period of time, and the standing and vibration steps may be repeated to make the concentration of the predetermined ions in the mixed solution uniform.
Next, in step S4, the concentration of the predetermined ion in the mixed solution per unit mass and the standard solution is determined.
In one example, a unit mass of the mixed solution, a standard solution, may be directly sampled and tested to determine the concentration of predetermined ions therein. The "unit mass" herein may be 1g, and may be other masses as long as the same mass is ensured in the samples extracted from the mixed solution and the standard solution.
In order to improve the test accuracy, in one example, a unit mass of the mixed solution and a unit mass of the standard solution may be taken from the mixed solution and the standard solution, respectively, the unit mass of the mixed solution and the unit mass of the standard solution may be fixed to the same volume, and the concentration of the predetermined ions in the fixed volume of the mixed solution and the standard solution may be measured, for example, as c1' and c2' and determining the concentration of the predetermined ion in the mixed solution per unit mass and the standard solution based on the measured concentrations of the predetermined ion in the mixed solution and the standard solution after the constant volume, for example, by measuring c1' and c2' is obtained by multiplying the volume of the fixed volume.
In one example, nitric acid may be added to the sampling solution to perform digestion of the organic solvent, and then a solvent such as water is added to dilute the sampling solution to a predetermined volume, for example, 100-2000 mL. The volume of the sampled mixed solution and the standard solution after constant volume is not particularly limited, and the mixed solution and the standard solution of unit mass can be diluted to the same volume and the ion concentration measurement accuracy can be ensured.
In one example, the ICP-OES spectrometer, the ion chromatograph, and other devices can be used to measure the concentration of the predetermined ions in the standard solution and the mixed solution after constant volume, and record the ion concentration (the unit of the ion concentration can be μ g/mL or mg/l) in the sample solution, and the content of the predetermined ions in the mixed solution and the standard solution per unit mass can be determined according to the measured concentration without performing a density test, thereby reducing the test error of the electrolyte content caused by the density test error.
Finally, in step S5, the electrolyte mass in the cell is determined, which can be determined by the following equation:
wherein m is1M is the mass of the electrolyte2Is the mass of the predetermined amount of the standard solution, c1Is a predetermined ion concentration in the mixed liquid per unit mass, c2Is the predetermined ion concentration in the standard solution per unit mass. As described above, in one example, m1、m2Can be in the unit of g, c1、c2The unit of (b) may be μ g/mL.
In one example, c in the above equation can be known by simple conversion2/c1C, the mixed solution and the standard solution measured in step S4 after the volume fixing2’/c1' equal, therefore, in step S5, c may be adopted2’/c1' substitution of c in the above formula2/c1Thereby improving the convenience of operation.
It can be seen that the determination method of the electrolyte content of the battery of the invention is convenient, the electrolyte content in the liquid battery can be calculated by directly using the test values of the standard solution and the mixed solution and the mass of the standard solution added into the battery, and the density test is not needed, so that the test error of the electrolyte content introduced by the density test error is reduced, and the data conversion is also not needed, for example, the test value (unit μ g/mL) is not needed to be converted into the concentration value (unit mol/L) for calculation. Meanwhile, compared with the prior art, the electrolyte content measuring method has many advantages, such as simplified test steps, no need of testing parallel samples, and accurate measurement of the electrolyte content of a single battery.
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is further described in detail with reference to the following embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
Example 1
(1) A pouch battery a was prepared, and in order to verify the feasibility of the present invention, the mass of the electrolyte in the pouch battery was previously determined to be 4 g.
(2) The method for measuring the quality of the electrolyte of the soft package battery A comprises the following specific steps:
s1: preparing a standard solution with the sodium ion concentration of 0.05 mol/L: dissolving sodium bis (fluorosulfonyl) imide (NaFSI) in an organic solvent, wherein the organic solvent is a mixture of Ethylene Carbonate (EC) and dimethyl carbonate (DMC) according to a mass ratio of 1:1, and adding 5.0g (m) of sodium bis (fluorosulfonyl) imide (NaFSI) into a soft-package battery A2) The standard solution is mixed with the electrolyte in the soft package battery to form a mixed solution, and the mixing is accelerated by using a vibration instrument;
s2: sampling by vibrating for 2h, standing for 12h and vibrating for 2h, and taking out a mixed solution to be tested;
s3: 1g of the standard solution and the mixed solution were taken, respectively. Digesting and fixing the volume to 100mL, and detecting the sodium ion concentration in the diluted sample liquid by using ICP-OES; the sodium ion concentration of the solution after the volume measurement is recorded and detected to be 9.58 mu g/mL (C)Sign board) And 5.26. mu.g/mL (C)Mixing of) (ii) a As analyzed previously, the electrolyte content (m) in the pouch cell can be calculated and determined using the following formula and converted1)：
According to the above formula, the mass m of the electrolyte1＝4.11g；
Calculating the error between the quality of the electrolyte of the soft package battery A obtained by the method and the original quality as follows: (4.11-4)/4 × 100% ═ 2.8%.
Example 2
(1) A pouch battery B in which the mass of the electrolyte was 9.6g was prepared.
(2) The method for measuring the quality of the electrolyte of the soft package battery B comprises the following specific steps:
s1: preparing a standard solution with the sodium ion concentration of 0.2 mol/L: dissolving NaTFSI in organic solvent, wherein the organic solvent is DMC solution, and adding 10.0g (m) of DMC solution into a soft package battery B2) The standard solution is mixed with the electrolyte in the soft package battery to form a mixed solution, and the mixing is accelerated by using a vibration instrument;
s2: sampling by shaking for 3h, standing for 12h and shaking for 3h, and taking out a mixed solution to be tested;
s3: 1g of the standard solution and the mixed solution were taken, respectively. Digesting and fixing the volume to 250mL, and detecting the sodium ion concentration in the diluted sample liquid by using ICP-OES; the sodium ion concentration of the solution after constant volume detection is recorded to be 15.33 mu g/mL (C)Sign board) And 7.89. mu.g/mL (C)Mixing of) (ii) a Calculating the electrolyte content in the soft package battery by adopting the following formula:
according to the above formula, the mass m of the electrolyte1＝9.43g；
Calculating the error between the quality of the electrolyte of the soft package battery B obtained by the method and the original quality: (9.43-9.6)/9.6 × 100% ═ 1.8%.
Example 3
(1) A cylindrical battery C in which the mass of the electrolyte was 7.8g was prepared.
(2) The method for measuring the quality of the electrolyte of the C cylindrical battery comprises the following specific steps:
s1: preparing a standard solution with the potassium ion concentration of 0.25 mol/L: dissolving potassium hexafluorophosphate in an organic solvent, wherein the organic solvent is a PC solution, adding 10.0g of a standard solution into a C cylindrical battery, mixing the standard solution with an electrolyte in the cylindrical battery to form a mixed solution, and accelerating the mixing by using a vibration meter;
s2: sampling by shaking for 3h, standing for 12h and shaking for 3h, and taking out a mixed solution to be tested;
s3: 1g of the standard solution and the mixed solution were taken, respectively. Digesting and fixing the volume to 500mL, and detecting the potassium ion concentration in the diluted sample liquid by using ICP-OES; recording the potassium ion concentration of the solution after the detection of constant volume to be 16.16 mu g/mL (C)Sign board) And 8.96. mu.g/mL (C)Mixing of) (ii) a Calculating the electrolyte content in the cylindrical battery using the following formula:
according to the above formula, the mass m of the electrolyte1＝8.04g；
Calculating the error between the electrolyte mass and the original mass of the cylindrical battery C obtained by the method of the invention: (8.04-7.8)/7.8 × 100% ═ 3.01%.
Example 4
(1) A square battery D in which the mass of the electrolyte was 12.0g was prepared.
(2) The method for measuring the quality of the electrolyte of the D-square battery comprises the following specific steps:
s1: preparing a standard solution with the potassium ion concentration of 0.5 mol/L: dissolving potassium hexafluorophosphate in an organic solvent, wherein the organic solvent is a PC solution, adding 13.0g of a standard solution into a D square battery, mixing the standard solution with an electrolyte in the square battery to form a mixed solution, and accelerating the mixing by using a vibration meter;
s2: sampling by vibrating for 4h, standing for 12h and vibrating for 4h, and taking out a mixed solution to be tested;
s3: 1g of the standard solution and the mixed solution were taken, respectively. Digesting to reach a constant volume of 1000mL, and detecting the potassium ion concentration in the diluted sample liquid by using ICP-OES; recording the potassium ion concentration of the solution after the detection of constant volume to be 16.10 mu g/mL (C)Sign board) And 8.45. mu.g/mL (C)Mixing of) (ii) a Calculating the electrolyte content in the square battery by adopting the following formula:
according to the above formula, the mass m of the electrolyte1＝11.77g；
Calculating the error between the electrolyte mass and the original mass of the square battery D obtained by the method of the invention: (11.77-12.0)/12.0 × 100% — 1.92%.
Example 5
(1) A square battery E in which the mass of the electrolyte was 20.0g was prepared.
(2) The method for measuring the quality of the electrolyte of the E-square battery comprises the following specific steps:
s1: preparing a standard solution with the potassium ion concentration of 1 mol/L: dissolving potassium bis (fluorosulfonyl) imide (KFSI) in an organic solvent, wherein the organic solvent is Ethyl Methyl Carbonate (EMC), adding 30.0g of standard solution into an E square battery, mixing the standard solution and electrolyte in the square battery to form a mixed solution, and accelerating the mixing by using a vibration meter;
s2: sampling by vibrating for 4h, standing for 24h and vibrating for 6h, and taking out a mixed solution to be tested;
s3: 1g of the standard solution and the mixed solution were taken, respectively. After digestion and volume fixing of 2000mL, detecting the potassium ion concentration in the diluted sample liquid by using ICP-OES; recording the potassium ion concentration of the solution after the detection of constant volume to be 16.14 mu g/mL (C)Sign board) And 9.78. mu.g/mL (C)Mixing of) (ii) a Calculating the electrolyte content in the square battery by adopting the following formula:
according to the above formula, the mass m of the electrolyte1＝19.51g；
Calculating the error between the electrolyte quality of the square battery E obtained by the method and the original quality: (19.51-20.0)/20.0 × 100% — 2.45%.
According to the specific implementation and test results of the embodiment 1, the embodiment 2, the embodiment 3, the embodiment 4 and the embodiment 5, the method provided by the invention is simple, the test result is high in accuracy and small in error (less than 5%), the method can be used for accurately detecting the electrolyte content in the battery, the operability is strong, and the method can be applied to various occasions, such as convenience and feasibility for distinguishing liquid batteries from solid-liquid batteries.
The foregoing is a more detailed description of the present invention in connection with specific preferred embodiments and is not intended to limit the practice of the invention to these embodiments. For those skilled in the art to which the invention pertains, several simple deductions or substitutions can be made without departing from the spirit of the invention, and all shall be considered as belonging to the protection scope of the invention.
Claims (9)
1. A method for determining the content of liquid electrolyte in a battery comprises the following steps:
s1, preparing a standard solution with preset ions, wherein the electrolyte does not contain the preset ions;
s2: preparing a battery needing to measure the content of the liquid electrolyte;
s3: adding a preset amount of standard solution into the battery, and mixing the standard solution with the liquid electrolyte in the battery to form a mixed solution;
s4: determining the concentration of the preset ions in the mixed solution and the standard solution of unit mass;
s5: determining an electrolyte mass in the battery, which is determined by the following equation:
wherein m is1M is the mass of the electrolyte2Is the mass of the predetermined amount of the standard solution, c1Is a predetermined ion concentration in the mixed liquid per unit mass, c2Is the predetermined ion concentration in the standard solution per unit mass.
2. The method of claim 1, wherein the predetermined ions contained in the standard solution are sodium ions, potassium ions, rubidium ions, cesium ions, bromide ions, chloride ions, or iodide ions.
3. The method for determining the content of a liquid electrolyte in a battery according to claim 2, wherein the concentration of the predetermined ions is equal to or greater than 0.001mol/L, preferably 0.05 to 1 mol/L.
4. The method for determining the content of the liquid electrolyte in the battery according to claim 2, wherein the standard solution is prepared by dissolving one of sodium bis (trifluorosulfonyl) imide, sodium bis (fluorosulfonyl) imide, sodium acetate, potassium hexafluorophosphate, potassium bis (trifluorosulfonyl) imide and potassium bis (fluorosulfonyl) imide in an organic solvent.
5. The method of claim 2, wherein the organic solvent is one or a mixture of two or more of Ethylene Carbonate (EC), Propylene Carbonate (PC), dimethyl carbonate (DMC), Ethyl Methyl Carbonate (EMC), diethyl carbonate (DEC) and a carboxylic acid ester organic solvent.
6. The method of claim 1, wherein in step S3, after the mixture is left for a period of time, the mixture is mixed with a vibrator or a rotator in an accelerated manner.
7. The method according to claim 1, wherein in step S4, the mixed solution and the standard solution are taken from the mixed solution and the standard solution respectively, the mixed solution and the standard solution are metered to the same volume, the concentrations of the predetermined ions in the mixed solution and the standard solution are measured after the metering, and the concentrations of the predetermined ions in the mixed solution and the standard solution are determined according to the measured concentrations of the predetermined ions in the mixed solution and the standard solution after the metering.
8. The method of claim 1, wherein the battery is a lithium ion battery or a sodium ion battery.
9. The method for determining the content of a liquid electrolyte in a battery according to claim 8, wherein the battery is any one of a pouch battery, a prismatic battery and a cylindrical battery.
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