CN110412102B - Method for determining additive content in lithium ion battery electrolyte - Google Patents
Method for determining additive content in lithium ion battery electrolyte Download PDFInfo
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Abstract
The invention discloses a method for determining the content of an additive in lithium ion battery electrolyte, which comprises the following steps: firstly, manufacturing and obtaining a plurality of standard sequence batteries; secondly, charging each standard sequence battery at constant current, and measuring voltage and capacity; thirdly, drawing a capacity differential curve of each standard sequence battery to obtain a reaction peak position and integrating to obtain reaction peak height and peak area data; fourthly, drawing a scatter diagram of the standard sequence battery, and fitting to obtain a quantitative relation between the quality of the additive and the reaction peak area or peak height data; fifthly, manufacturing an electrolyte battery to be tested for the electrolyte to be tested with the additive to be tested; and sixthly, drawing a capacity differential curve of the electrolyte battery to be measured to obtain a reaction peak position, integrating to obtain reaction peak height and peak area data, and calculating the quality of the additive with the content to be measured. The method can accurately and reliably measure the content of the additive in the lithium ion battery electrolyte.
Description
Technical Field
The invention relates to the technical field of lithium ion batteries, in particular to a method for determining the content of an additive in an electrolyte of a lithium ion battery.
Background
At present, lithium ion batteries have been widely used in the fields of digital products, electric vehicles and energy storage due to their advantages of high energy density, good cycle performance, green and no pollution. The electrolyte is used as an important component of the lithium ion battery, wherein a trace amount of additive plays a crucial role in improving the performance of the battery.
In the prior art, a conventional method for analyzing the components of an electrolyte of a lithium ion battery includes: gas chromatography, gas chromatography-mass spectrometry, ion chromatography, and the like. The gas chromatography and the gas chromatography-mass spectrometry are combined, and are suitable for detecting organic components in the electrolyte, and the ion chromatography is suitable for detecting inorganic salts. The existing methods can meet the analysis requirements of most of lithium ion battery electrolytes with formulas, but for some electrolyte additive components with high boiling points, thermal decomposition and sensitivity to water, the conventional methods are often poor in reproducibility, so that the test error is large.
Therefore, there is an urgent need to develop a method for accurately and reliably measuring the content of the additive in the electrolyte of the lithium ion battery.
Disclosure of Invention
The invention aims to provide a method for measuring the content of an additive in a lithium ion battery electrolyte, aiming at the technical defects in the prior art.
Therefore, the invention provides a method for determining the content of an additive in lithium ion battery electrolyte, which comprises the following steps:
firstly, respectively adding additives with preset different contents into a plurality of preset electrolytes with known components to correspondingly obtain a plurality of standard sequence electrolytes, and respectively manufacturing a plurality of standard sequence batteries by using the plurality of standard sequence electrolytes;
secondly, performing constant current charging on each standard sequence battery by using current with a preset magnitude, and measuring to obtain battery voltage and battery capacity data of each standard sequence battery in the constant current charging process;
differentiating the battery voltage V by using the battery capacity Q of the standard sequence battery for each standard sequence battery, calculating to obtain dQ/dV, then drawing a capacity differential curve of each standard sequence battery by using the battery voltage of the standard sequence battery as an abscissa and the dQ/dV as an ordinate to obtain a reaction peak position of the additive in each standard sequence battery, and obtaining the reaction peak height and peak area data of the additive by integration;
fourthly, for the plurality of standard sequence batteries, drawing scatter diagrams of the additives in the plurality of standard sequence batteries by taking the content of the additives in the standard sequence batteries as a vertical coordinate and taking the reaction peak area or peak height data of the additives in each standard sequence battery as a horizontal coordinate, and fitting the scatter diagrams to obtain a quantitative relational expression between the quality of the additives and the reaction peak area or peak height data;
fifthly, manufacturing an electrolyte battery to be tested by adopting the same manufacturing method as the standard sequence battery manufactured in the first step for a part of electrolyte to be tested with the additive to be tested;
and sixthly, performing constant current charging on the electrolyte battery to be measured by using current with a preset magnitude, measuring to obtain battery voltage and battery capacity data of the electrolyte battery to be measured in the constant current charging process, then differentiating the battery voltage V by using the battery capacity Q of the electrolyte battery to be measured to obtain dQ/dV through calculation, then drawing a capacity differential curve of the electrolyte battery to be measured by using the battery voltage of the electrolyte battery to be measured as a horizontal coordinate and using the dQ/dV as a vertical coordinate to obtain a reaction peak position of the additive with the content to be measured, obtaining the reaction peak height and peak area data of the additive with the content to be measured through integration, and then calculating the quality of the additive with the content to be measured in the electrolyte to be measured according to the quantitative relational expression obtained in the fourth step.
Wherein, after the sixth step, the following steps are further included:
and seventhly, calculating to obtain the mass content of the additive in the electrolyte to be detected according to the liquid injection amount of the electrolyte to be detected when the electrolyte battery to be detected is manufactured by the electrolyte to be detected and the mass of the additive with the content to be detected in the electrolyte to be detected obtained in the fifth step.
The electrolyte comprises a solute and a solvent, wherein the solute is lithium hexafluorophosphate LiPF6The solvent comprises: dimethyl carbonate DMC, methyl ethyl carbonate EMC and ethylene carbonate EC, the mass ratio of dimethyl carbonate DMC, methyl ethyl carbonate EMC and ethylene carbonate EC is 3:3:4, and lithium hexafluorophosphate LiPF6The molar concentration of (A) is 1.2 mol/L.
Wherein, in the second step and the sixth step, the current with the preset magnitude is 0.02C-0.05C.
In the fourth step, the quantitative relation is specifically as follows:
y is kx + b, wherein x is the area of the additive reaction peak or the peak height response value in the standard sequence battery; y is the mass of the additive in g; k and b are constants, k is the slope of a straight line connecting the scatter points in the scatter diagram, and b is the intersection point of the straight line connecting the scatter points in the scatter diagram and the y axis.
Compared with the prior art, the method for determining the content of the additive in the lithium ion battery electrolyte can accurately and reliably measure the content of the additive in the lithium ion battery electrolyte, and has great practical significance.
Drawings
FIG. 1 is a flow chart of a method for determining the content of an additive in an electrolyte of a lithium ion battery according to the present invention;
FIG. 2 is a schematic diagram of capacity differential curves of a plurality of standard series batteries in example 1 according to a method for determining the content of an additive in an electrolyte of a lithium ion battery provided by the present invention;
FIG. 3 is a schematic diagram of a data fitting scatter plot between peak-height response values and mass of additives in a plurality of standard sequence batteries of example 1 according to the method for determining the content of the additives in the electrolyte of a lithium ion battery provided by the present invention; in the figure, the relation is fitted: x is the peak height response value, and y is the mass of the additive;
fig. 4 is a schematic diagram of a capacity differential curve of the electrolyte battery to be measured in example 1, which is a method for measuring the content of the additive in the electrolyte of the lithium ion battery provided by the present invention.
Detailed Description
In order that those skilled in the art will better understand the technical solution of the present invention, the following detailed description of the present invention is provided in conjunction with the accompanying drawings and embodiments.
Referring to fig. 1, the invention provides a method for determining the content of an additive in an electrolyte of a lithium ion battery, which comprises the following steps:
firstly, respectively adding additives with preset different contents into a plurality of preset electrolytes with known components to correspondingly obtain a plurality of standard sequence electrolytes, and respectively manufacturing a plurality of standard sequence batteries by using the plurality of standard sequence electrolytes;
secondly, performing constant current charging on each standard sequence battery by using a current with a preset magnitude (for example, a small current of 0.02C-0.05C), and measuring to obtain battery voltage and battery capacity data of each standard sequence battery in the constant current charging process;
differentiating the battery voltage V by using the battery capacity Q of the standard sequence battery for each standard sequence battery, calculating to obtain dQ/dV, then drawing a capacity differential curve of each standard sequence battery by using the battery voltage of the standard sequence battery as an abscissa and the dQ/dV as an ordinate to obtain a reaction peak position (namely, an abscissa voltage value position corresponding to the maximum peak height value of the reaction peak) of the additive in each standard sequence battery, and obtaining the reaction peak height and peak area data of the additive through integration;
fourthly, for the plurality of standard sequence batteries, drawing scatter diagrams of the additives in the plurality of standard sequence batteries by taking the content (namely different preset content) of the additives in the standard sequence batteries as a vertical coordinate and taking the reaction peak area or peak height data of the additives in each standard sequence battery as a horizontal coordinate, and fitting the scatter diagrams to obtain a quantitative relational expression between the quality of the additives and the reaction peak area or peak height data;
fifthly, for a part of electrolyte to be detected with the additive to be detected, manufacturing the electrolyte battery to be detected by adopting the same manufacturing method (only different electrolytes, namely referring to the preparation step of the first step) as the standard sequence battery manufactured in the first step;
sixthly, performing constant current charging on the electrolyte battery to be measured by using a current with a preset magnitude (for example, a small current of 0.02C-0.05C), measuring to obtain the battery voltage and battery capacity data of the electrolyte battery to be measured in the constant current charging process, then, the battery voltage V is differentiated by the battery capacity Q of the electrolyte battery to be measured, dQ/dV is obtained by calculation, then, taking the battery voltage of the electrolyte battery to be measured as an abscissa and the dQ/dV as an ordinate, drawing a capacity differential curve of the electrolyte battery to be measured to obtain a reaction peak position (namely, an abscissa voltage value position corresponding to the maximum peak height value of the reaction peak) of the additive with the content to be measured, and obtaining the reaction peak height and peak area data of the additive with the content to be measured by integration, and then calculating the quality of the additive with the content to be measured in the electrolyte to be measured according to the quantitative relation obtained in the fourth step.
For the present invention, after the sixth step, the following steps are further included:
and seventhly, calculating to obtain the mass content (namely mass percentage) of the additive in the electrolyte to be detected according to the liquid injection amount of the electrolyte to be detected when the electrolyte battery to be detected is manufactured by the electrolyte to be detected and the mass of the additive with the content to be detected in the electrolyte to be detected obtained in the fifth step.
As for the fifth step, it should be noted that, for the electrolyte battery to be tested, as described above, with reference to the second step and the third step, the additive to be tested is qualitatively determined according to the reaction peak position, and the reaction peak area or the peak height response value of the additive in the electrolyte to be tested is obtained.
In the first step, specifically, a conventional lithium ion battery electrolyte and a solvent are used to prepare a predetermined electrolyte with known components, i.e., a basic electrolyte.
In the first step, a plurality of portions of a predetermined electrolyte of known composition, each portion being identical, is embodied. The preset electrolyte with known components can be any existing lithium ion battery electrolyte, and specifically comprises a solute and a solventAn agent, wherein the solute is lithium hexafluorophosphate LiPF6The solvent comprises: dimethyl carbonate DMC, methyl ethyl carbonate EMC and ethylene carbonate EC, the mass ratio of dimethyl carbonate DMC, methyl ethyl carbonate EMC and ethylene carbonate EC is 3:3:4, and lithium hexafluorophosphate LiPF6The molar concentration of (A) is 1.2 mol/L.
In the first step, it is noted that the additive is a known specific kind of additive, for example, the additive LiODFB.
In the first step, it is to be noted that a standard sequence battery is manufactured by using a standard sequence electrolyte and adopting a conventional lithium ion battery preparation process, and the standard sequence battery is a lithium ion battery; for example, the following preparation steps may be included:
firstly, manufacturing a positive plate: mixing a positive active substance, a conductive agent and a binder according to a preset mass ratio, uniformly dispersing the mixture in a solvent to prepare a positive slurry, uniformly coating the positive slurry on the surface of a positive current collector (such as an aluminum foil), sequentially performing the working procedures of rolling, shearing and dedusting, and welding a positive electrode lug to obtain a positive electrode piece;
and then, manufacturing a negative plate: and then, manufacturing a negative plate: mixing a negative active material, a conductive agent and a binder according to a preset mass ratio, uniformly dispersing the mixture in a solvent to prepare a negative slurry, uniformly coating the negative slurry on the surface of a negative current collector (such as a copper foil), sequentially performing the working procedures of rolling, shearing and dedusting, and welding a negative electrode lug to obtain a negative electrode pole piece;
then, manufacturing a battery pole group: winding the positive plate, the diaphragm and the negative plate together, and ending the negative plate to manufacture a cylindrical battery pole group;
then, assembling the battery: assembling a battery pole into a shell, injecting a non-aqueous electrolyte (specifically a standard sequence electrolyte), and then sealing to obtain an assembled lithium ion battery, namely the standard sequence battery;
the positive electrode active material, the negative electrode active material, the conductive agent, and the binder may be any of those materials and the ratios of the components that are conventionally used.
In the second step, specifically, during constant current charging, the cut-off voltage of the standard series battery can be adjusted according to the reaction potential of the measured additive, and can also be uniformly set to be 3.3V.
In the third step, in concrete implementation, according to the graph, the integration processing of the peak height and the peak area is performed, and the concrete processing manner is similar to the prior art, and the detailed description is not provided herein. For example, it may be: integration was performed using origin software available from OriginLab corporation to obtain the peak height and peak area in the capacity differential curve plot of the standard sequence battery. In the present invention, since integration is performed by origin software, detailed description is not provided herein, and of course, other existing integration methods may be adopted as long as calculation of the peak area and the peak height of each peak in one curve can be achieved.
In the present invention, in a specific implementation, in the fourth step, the quantitative relation is specifically as follows:
y is kx + b, wherein x is the area of the additive reaction peak or the peak height response value in the standard sequence battery; y is the mass of the additive in g; k and b are constants, k is the slope of a straight line connecting the scatter points in the scatter diagram, and b is the intersection point of the straight line connecting the scatter points in the scatter diagram and the y axis.
In the present invention, the voltage value, which is the reaction peak position, in the curve plotted with the cell voltage as the abscissa and the dQ/dV as the ordinate can be used as a basis for qualitative analysis of different types of additives.
In the invention, in a curve drawn by taking the battery voltage as an abscissa and the dQ/dV as an ordinate, the peak height and the peak area are taken as the basis for quantitative analysis of the additive.
In order to more clearly understand the technical solution of the present invention, the technical solution of the present invention is described below by specific examples.
Example 1.
The electrolyte containing the additive LiODFB is taken as an example, and the invention is described in detail with reference to the accompanying drawings so as to further illustrate the essential characteristics of the invention. In this example, the method of the present invention was used to detect the content of the additive LiODFB in the electrolyte.
Firstly, preparing four parts of basic electrolyte (DMC: EMC: EC is 3:3:4, LiPF6 of 1.2 mol/L) by using the electrolyte and solvent of a conventional lithium ion battery, adding additives to be tested LiODFB with different contents to obtain four parts of standard sequence electrolyte, respectively preparing four 18650 type standard sequence batteries by using the sequence electrolyte, recording the adding amount of the electrolyte, and recording data as shown in Table 1.
Table 1: standard sequence battery liquid injection amount and additive content data table.
And secondly, performing constant current charging on the four obtained standard sequence batteries at a low current of 0.05C, setting the cut-off voltage to be 3.0V, and obtaining voltage and capacity data in the battery charging process.
And thirdly, for the standard sequence battery, carrying out differential calculation on the voltage by using the battery capacity to obtain dQ/dV, and drawing a capacity differential curve of the battery by using the battery voltage as an abscissa and using the dQ/dV as an ordinate, as shown in fig. 2. The reaction peak position of the additive LiODFB was obtained as 1.97V, and peak height data were obtained by integration, as shown in table 2.
Table 2: data table of LiODFB reaction peak position and peak height in standard sequence battery.
| Sample numbering | Mass of additive/g | Peak position/V of reaction | Peak height response value |
| 1 | 0.0411 | 1.97 | 66.04 |
| 2 | 0.0273 | 1.98 | 44.31 |
| 3 | 0.0139 | 1.97 | 26.66 |
| 4 | 0.0046 | 1.98 | 16.25 |
And fourthly, drawing a scatter diagram by taking the content of the additive in the standard sequence battery as a vertical coordinate and the reaction peak height data of the additive as a horizontal coordinate, and obtaining a quantitative fitting relation between the mass y of the additive and the reaction peak height response value x as shown in figure 3: 0.00072898 x-0.00619403.
And fifthly, referring to the first step, manufacturing the electrolyte battery to be tested by using the electrolyte to be tested, and recording the liquid injection amount of the battery to be 4.78 g. And referring to the second and third steps, a capacity differential curve of the electrolyte battery to be tested is obtained, as shown in fig. 4, and a reaction peak position and a peak height response value of the additive in the electrolyte to be tested are obtained, as shown in table 3.
Table 3: and the additive reaction peak position and peak height data table of the electrolyte battery to be tested.
| Sample numbering | Electrolyte injection amount/g | Peak position/V of reaction | Peak height response value |
| 5 | 4.81 | 1.97 | 50.21 |
In the examples, the quantitative fit relationship between the mass y of the additive and the peak-to-peak response x of the reaction peak obtained in the fourth step is: and y is 0.00072898x-0.00619403, and the mass of the additive in the electrolyte to be measured is calculated to be 0.00072898x 50.21-0.00619403 g which is 0.0304 g. Then, the LiODFB content in the electrolyte to be measured is calculated to be 0.0304/4.81 multiplied by 100 percent to be 0.63 percent according to the liquid injection amount of the battery being 4.81 g.
The detection method provided by the invention is not limited to the detection of the content of the film-forming additive of the lithium ion battery electrolyte, and the development of the corresponding test method can be carried out based on the idea provided by the invention in the detection of other components participating in the reaction. Any equivalent alterations to the present invention are intended to be within the scope of the present invention.
Based on the technical scheme, the method for determining the content of the additive in the lithium ion battery electrolyte is used for drawing a capacity differential curve based on the voltage and capacity data of the first charging of the battery. Different additives have electrochemical reaction with the electrode under different voltages, so that qualitative analysis can be carried out on the additives according to the reaction peak position, namely the voltage value. Meanwhile, in view of the fact that the higher the content of the additive is, the larger the reaction peak area and the peak height of the capacity differential curve are, the quantitative analysis purpose of the additive is finally achieved by establishing a quantitative relation between the reaction peak area or the peak height and the quality of the additive.
The method provided by the invention does not need a high-sensitivity analysis instrument and pretreatment of the electrolyte, and directly analyzes and calculates the battery charging test data, and the test result is accurate and reliable, so the method has practical popularization significance in the lithium ion battery industry.
In summary, compared with the prior art, the method for determining the content of the additive in the lithium ion battery electrolyte provided by the invention can accurately and reliably measure the content of the additive in the lithium ion battery electrolyte, and has great practical significance.
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and decorations can be made without departing from the principle of the present invention, and these modifications and decorations should also be regarded as the protection scope of the present invention.
Claims (5)
1. A method for measuring the content of an additive in lithium ion battery electrolyte is characterized by comprising the following steps:
firstly, respectively adding additives with preset different contents into a plurality of preset electrolytes with known components to correspondingly obtain a plurality of standard sequence electrolytes, and respectively manufacturing a plurality of standard sequence batteries by using the plurality of standard sequence electrolytes;
secondly, performing constant current charging on each standard sequence battery by using current with a preset magnitude, and measuring to obtain battery voltage and battery capacity data of each standard sequence battery in the constant current charging process;
differentiating the battery voltage V by using the battery capacity Q of the standard sequence battery for each standard sequence battery, calculating to obtain dQ/dV, then drawing a capacity differential curve of each standard sequence battery by using the battery voltage of the standard sequence battery as an abscissa and the dQ/dV as an ordinate to obtain a reaction peak position of the additive in each standard sequence battery, and obtaining the reaction peak height and peak area data of the additive by integration;
fourthly, for the plurality of standard sequence batteries, drawing scatter diagrams of the additives in the plurality of standard sequence batteries by taking the content of the additives in the standard sequence batteries as a vertical coordinate and taking the reaction peak area or peak height data of the additives in each standard sequence battery as a horizontal coordinate, and fitting the scatter diagrams to obtain a quantitative relational expression between the quality of the additives and the reaction peak area or peak height data;
fifthly, manufacturing an electrolyte battery to be tested by adopting the same manufacturing method as the standard sequence battery manufactured in the first step for a part of electrolyte to be tested with the additive to be tested;
and sixthly, performing constant current charging on the electrolyte battery to be measured by using current with a preset magnitude, measuring to obtain battery voltage and battery capacity data of the electrolyte battery to be measured in the constant current charging process, then differentiating the battery voltage V by using the battery capacity Q of the electrolyte battery to be measured to obtain dQ/dV through calculation, then drawing a capacity differential curve of the electrolyte battery to be measured by using the battery voltage of the electrolyte battery to be measured as a horizontal coordinate and using the dQ/dV as a vertical coordinate to obtain a reaction peak position of the additive with the content to be measured, obtaining the reaction peak height and peak area data of the additive with the content to be measured through integration, and then calculating the quality of the additive with the content to be measured in the electrolyte to be measured according to the quantitative relational expression obtained in the fourth step.
2. The assay of claim 1, further comprising, after the sixth step, the steps of:
and seventhly, calculating to obtain the mass content of the additive in the electrolyte to be detected according to the liquid injection amount of the electrolyte to be detected when the electrolyte battery to be detected is manufactured by the electrolyte to be detected and the mass of the additive with the content to be detected in the electrolyte to be detected obtained in the fifth step.
3. The method of claim 1The determination method is characterized in that the preset electrolyte with known components specifically comprises a solute and a solvent, wherein the solute is lithium hexafluorophosphate LiPF6The solvent comprises: dimethyl carbonate DMC, methyl ethyl carbonate EMC and ethylene carbonate EC, the mass ratio of dimethyl carbonate DMC, methyl ethyl carbonate EMC and ethylene carbonate EC is 3:3:4, and lithium hexafluorophosphate LiPF6The molar concentration of (A) is 1.2 mol/L.
4. The measuring method according to claim 1, wherein the current of the predetermined magnitude is 0.02C to 0.05C in the second step and the sixth step.
5. The assay of any one of claims 1 to 4, wherein in the fourth step, the quantitative relationship is specified by:
y is kx + b, wherein x is the area of the additive reaction peak or the peak height response value in the standard sequence battery; y is the mass of the additive in g; k and b are constants, k is the slope of a straight line connecting the scatter points in the scatter diagram, and b is the intersection point of the straight line connecting the scatter points in the scatter diagram and the y axis.
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