CN114487056A - Electrode material consistency determination method, system, electronic device, and storage medium - Google Patents
Electrode material consistency determination method, system, electronic device, and storage medium Download PDFInfo
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Abstract
The application discloses an electrode material consistency determination method, an electrode material consistency determination system, electronic equipment and a storage medium. The electrode material consistency judging method comprises the following steps: carrying out multiple electrochemical tests on the material to be tested to obtain multiple groups of test parameter sets; determining a target voltage parameter range from any one group of test parameter sets, and taking at least one candidate voltage parameter in the target voltage parameter range as a first target parameter; obtaining the candidate current parameter corresponding to the first target parameter from a plurality of groups of the test parameter sets, and taking the candidate current parameter as a second target parameter; calculating according to the plurality of second target parameters to obtain a judgment parameter; and comparing the judgment parameters with preset reference parameters, and judging the consistency of the material to be detected according to the comparison result. The method and the device can avoid testing the multiple parameter indexes of the material to be tested, so that the judgment efficiency of the consistency of the material to be tested is improved.
Description
Technical Field
The present disclosure relates to the field of consistency determination technologies, and in particular, to a method and a system for determining consistency of an electrode material, an electronic device, and a storage medium.
Background
At present, with the increasing shortage of fossil energy resources, energy storage devices such as batteries and capacitors are widely used in various fields. Among them, the negative electrode material, the positive electrode material, and the like are important components of the energy storage device.
Taking the negative electrode material as an example, in the related art, when the consistency of the negative electrode material is determined, multiple parameter indexes such as particle size distribution, specific surface area, tap density, morphology, crystal structure and the like of the negative electrode material need to be detected, and the consistency of the negative electrode material is determined according to detection results of the multiple parameter indexes, that is, the method cannot obtain a determination conclusion through a single test item index, so that the consistency determination efficiency is influenced.
Disclosure of Invention
The present application is directed to solving at least one of the problems in the prior art. Therefore, the application provides an electrode material consistency determination method, an electrode material consistency determination system, an electronic device and a storage medium, which can avoid testing multiple parameter indexes of a material to be tested, so that the consistency determination efficiency of the material to be tested is improved.
The electrode material consistency determination method according to an embodiment of the first aspect of the present application includes: carrying out multiple electrochemical tests on the material to be tested to obtain multiple groups of test parameter sets; wherein the electrochemical test comprises a CV test or an LSV test; each group of the test parameter sets comprises a plurality of candidate current parameters and candidate voltage parameters corresponding to the candidate current parameters; determining a target voltage parameter range from any one group of test parameter sets, and taking at least one candidate voltage parameter in the target voltage parameter range as a first target parameter; obtaining the candidate current parameter corresponding to the first target parameter from a plurality of groups of test parameter groups, and taking the candidate current parameter as a second target parameter; calculating according to the plurality of second target parameters to obtain a judgment parameter; and comparing the judgment parameters with preset reference parameters, and judging the consistency of the material to be detected according to the comparison result.
The electrode material consistency judging method provided by the embodiment of the application has at least the following beneficial effects: the electrochemical test is carried out on the material to be tested to obtain a plurality of groups of test parameter sets, and a target voltage parameter range capable of providing a judgment basis for consistency is obtained from any one group of test parameter sets. And obtaining a second target parameter according to the first target parameter in the target voltage parameter range, and obtaining a judgment parameter according to a plurality of second target parameters, so as to determine the consistency of the material to be detected according to the comparison result of the judgment parameter and the reference parameter. Therefore, the electrode material consistency determination method provided by the embodiment of the application avoids detecting multiple parameter indexes of the material to be detected, and only needs to extract target parameters (including a first target parameter and a second target parameter) from a test parameter group corresponding to an electrochemical test to obtain the determination parameters. Therefore, the electrode material consistency determination method provided by the embodiment of the application improves consistency determination efficiency.
According to some embodiments of the present application, the set of test parameters includes a candidate parameter range representing a non-oxidation peak range, a non-reduction peak range; the determining a target voltage parameter range from any one set of the test parameter sets comprises: and taking the candidate parameter range of any one group of the test parameter groups as the target voltage parameter range.
According to some embodiments of the present application, the performing multiple sets of electrochemical tests on the material to be tested to obtain multiple sets of test parameters includes: performing CV test or LSV test according to a preset scanning speed to obtain a plurality of candidate current parameters and a plurality of candidate voltage parameters; obtaining a group of test parameter sets according to the candidate current parameters and the candidate voltage parameters; and adjusting the scanning speed, and executing the scanning operation according to the preset scanning speed again to obtain a plurality of groups of test parameter sets.
According to some embodiments of the present application, the calculating a decision parameter according to a plurality of second target parameters includes: acquiring the scanning speed corresponding to the second target parameter; in the same scanning direction, calculating to obtain the judgment parameter according to the plurality of second target parameters and the corresponding scanning speed; wherein the same scanning direction includes any one of the candidate voltage parameter increasing direction and the candidate voltage parameter decreasing direction.
According to some embodiments of the application, the determining the consistency of the material to be tested according to the comparison result includes: if the comparison result shows that the judgment parameter is equal to the reference parameter, judging that the consistency of the material to be detected is a first level; and if the comparison result shows that the judgment parameter is not equal to the reference parameter, judging that the consistency of the material to be detected is a second level.
According to some embodiments of the application, the determining the consistency of the material to be tested according to the comparison result includes: if the comparison result shows that the judgment parameter is not equal to the reference parameter, acquiring a difference value between the judgment parameter and the reference parameter; and if the difference value is within a preset range, judging that the consistency of the material to be detected is a preset grade corresponding to the preset range.
An electrode material consistency determination system according to an embodiment of a second aspect of the present application includes: the test module is used for carrying out multiple electrochemical tests on the material to be tested to obtain multiple groups of test parameter sets; wherein the electrochemical test comprises a CV test or an LSV test; each group of the test parameter sets comprises a plurality of candidate current parameters and candidate voltage parameters corresponding to the candidate current parameters; a first query module, configured to determine a target voltage parameter range from any one of the sets of test parameters, and use at least one candidate voltage parameter in the target voltage parameter range as a first target parameter; the second query module is used for obtaining the candidate current parameter corresponding to the first target parameter from a plurality of groups of test parameter sets and taking the candidate current parameter as a second target parameter; the calculation module is used for calculating to obtain a judgment parameter according to the plurality of second target parameters; and the judging module is used for comparing the judging parameters with preset reference parameters and judging the consistency of the material to be detected according to the comparison result.
According to some embodiments of the application, further comprising: the device comprises a testing device, a detection device and a control device, wherein the testing device is a three-electrode electrochemical system or a two-electrode electrochemical system; the preparation material of the working electrode of the testing device is the material to be tested; the test module is used for carrying out the electrochemical test on the test device for a plurality of times.
An electronic device according to an embodiment of a third aspect of the present application includes: at least one processor; at least one memory for storing at least one program; when the at least one program is executed by the at least one processor, the at least one processor is caused to implement the electrode material consistency determination method according to the first aspect.
A computer-readable storage medium according to an embodiment of the fourth aspect of the present application, wherein processor-executable instructions are stored, which when executed by a processor, are used for implementing the electrode material consistency determination method according to the first aspect.
According to the electrode material consistency judging method, the system, the electronic equipment and the storage medium, electrochemical testing is carried out on the material to be detected, and a third candidate parameter range corresponding to a non-Faraday capacitance characteristic signal area in a testing parameter group is selected as a target voltage parameter range, so that a judging parameter capable of representing consistency change of the material to be detected is obtained according to the target voltage parameter range, and qualitative judgment and/or quantitative judgment on the consistency of the material to be detected is further realized according to a comparison result of the judging parameter and a reference parameter. Therefore, the embodiment of the application avoids testing multiple parameter indexes of the material to be tested, and improves the judgment efficiency of the consistency of the material to be tested.
Additional aspects and advantages of the present application will be set forth in part in the description which follows and, in part, will be obvious from the description, or may be learned by practice of the present application.
Drawings
The present application is further described with reference to the following figures and examples, in which:
fig. 1 is a schematic flow chart of a method for determining consistency of electrode materials according to an embodiment of the present disclosure;
FIG. 2 is a schematic diagram showing a CV curve of 0.5mV/s as the scanning speed in the example of the present application;
FIG. 3 is another schematic flow chart illustrating a method for determining consistency of electrode materials according to an embodiment of the present disclosure;
FIG. 4 is another schematic flow chart of a method for determining consistency of electrode materials according to an embodiment of the present disclosure;
FIG. 5 is a schematic diagram of a candidate current parameter-scan speed curve with 2.5V as a first target parameter according to an embodiment of the present invention;
FIG. 6 is another schematic flow chart illustrating a method for determining consistency of electrode materials according to an embodiment of the present disclosure;
FIG. 7 is another schematic flow chart illustrating a method for determining consistency of electrode materials according to an embodiment of the present disclosure;
fig. 8 is a block diagram of an electrode material consistency determination system according to an embodiment of the present disclosure.
Detailed Description
Reference will now be made in detail to embodiments of the present application, examples of which are illustrated in the accompanying drawings, wherein like or similar reference numerals refer to the same or similar elements or elements having the same or similar function throughout. The embodiments described below with reference to the drawings are exemplary only for the purpose of explaining the present application and are not to be construed as limiting the present application.
In the description of the present application, it is to be understood that the positional descriptions, such as the directions of up, down, front, rear, left, right, etc., referred to herein are based on the directions or positional relationships shown in the drawings, and are only for convenience of description and simplification of description, and do not indicate or imply that the referred device or element must have a specific direction, be constructed and operated in a specific direction, and thus, should not be construed as limiting the present application.
In the description of the present application, the meaning of a plurality is one or more, the meaning of a plurality is two or more, and the above, below, exceeding, etc. are understood as excluding the present number, and the above, below, within, etc. are understood as including the present number. If the first and second are described for the purpose of distinguishing technical features, they are not to be understood as indicating or implying relative importance or implicitly indicating the number of technical features indicated or implicitly indicating the precedence of the technical features indicated.
In the description of the present application, unless otherwise expressly limited, terms such as set, mounted, connected and the like should be construed broadly, and those skilled in the art can reasonably determine the specific meaning of the terms in the present application by combining the detailed contents of the technical solutions.
In the description of the present application, reference to the description of the terms "one embodiment," "some embodiments," "an illustrative embodiment," "an example," "a specific example," or "some examples," etc., means that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the present application. In this specification, the schematic representations of the terms used above do not necessarily refer to the same embodiment or example. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples.
First, several terms referred to in the present application are explained:
the electrochemical test is a process of applying disturbance or stimulation to an electrochemical system based on an electrochemical theory, recording or observing the electrochemical response of the electrochemical system, and analyzing the electrochemical response to obtain the characteristics, the performance, the behavior and other specificities of the electrochemical system.
The electrochemical system comprises a working electrode, an auxiliary electrode, a reference electrode, a diaphragm, an electrolyte (or electrolyte) and the like. Wherein, the working electrode means that the reaction to be studied takes place on this electrode; the auxiliary electrode is an electrode which forms a loop with the working electrode; the reference electrode is an electrode having a relatively stable and known potential and is used to provide a voltage monitoring reference for the working electrode.
CV test (cyclic voltammetry test) which controls the electrode voltage sweep at different rates and records a test method of current-voltage curves. Wherein the voltage range includes a plurality of voltages at which different reduction reactions and oxidation reactions alternately occur at the electrode. The reversibility of electrode reaction, the possibility of adsorption of intermediate and phase boundary or formation of new phase, the property of coupling chemical reaction, etc. can be judged according to the shape of the current-voltage curve.
The LSV test (linear sweep voltammetry test) refers to a test method in which a linear potential sweep (a linear relationship of potential with time) is applied between a working electrode and an auxiliary electrode.
In the following embodiments, the negative electrode material to be measured is taken as an example of the material to be measured, and the electrode material includes any one of a negative electrode material and a positive electrode material. However, it should be understood that when the positive electrode material to be measured is used as the material to be measured, the following embodiments may be adapted to fall within the scope of the present application.
Referring to fig. 1 and 2, the present application provides an electrode material consistency determination method, which includes, but is not limited to, steps S110 to S150:
s110, carrying out multiple electrochemical tests on the negative electrode material to be tested to obtain multiple groups of test parameter sets; wherein the electrochemical test comprises a CV test or an LSV test; each group of test parameter group comprises a plurality of candidate current parameters and candidate voltage parameters corresponding to the candidate current parameters;
s120, determining a target voltage parameter range from any group of test parameter sets, and taking at least one candidate voltage parameter in the target voltage parameter range as a first target parameter;
s130, obtaining candidate current parameters corresponding to the first target parameters from multiple groups of test parameter sets, and taking the candidate current parameters as second target parameters;
s140, calculating to obtain a judgment parameter according to the plurality of second target parameters;
s150, comparing the judgment parameters with preset reference parameters, and judging the consistency of the anode material to be detected according to the comparison result.
Specifically, the anode material to be tested is used as a reaction research object, and an electrochemical test such as a CV test or an LSV test is performed on an electrochemical system to be tested composed of the anode material to be tested under different test conditions. Taking a CV test as an example, a plurality of candidate voltage parameters in the test and a candidate current parameter corresponding to each candidate voltage parameter are recorded, and a plurality of candidate voltage parameters and a plurality of candidate current parameters under the same test condition are combined into a group of test parameter groups, so that a plurality of groups of test parameter groups are obtained. A corresponding CV curve (i.e., a candidate current parameter-candidate voltage parameter curve) is constructed according to each set of test parameter sets, and a target voltage parameter range is determined from any one set of test parameter sets, i.e., a target voltage parameter range is determined from any one CV curve. The target voltage parameter range represents a range formed by a plurality of candidate voltage parameters corresponding to an effective area in a CV curve, and the effective area refers to an area capable of providing a judgment basis for the consistency of the anode material to be detected. Selecting any candidate voltage parameter from the range of the target voltage parameters as a first target parameter, searching a candidate current parameter corresponding to the first target parameter from each group of test parameter sets, and taking the candidate current parameter as a second target parameter so as to obtain a plurality of second target parameters. And calculating to obtain a judgment parameter for representing the current consistency of the negative electrode material to be detected according to the plurality of second target parameters, comparing the judgment parameter with a reference parameter of a reference electrochemical system, and judging the consistency of the negative electrode material to be detected according to a comparison result so as to obtain a judgment conclusion that the consistency is 'good, medium and poor'. It is understood that the reference electrochemical system includes a reference anode material, which is the subject of the reaction study. And under the same test condition, performing CV test or LSV test on the reference electrochemical system, which is the same as that of the electrochemical system to be tested, and calculating to obtain reference parameters according to the same method.
According to the electrode material consistency judging method provided by the embodiment of the application, a plurality of groups of testing parameter sets are obtained by performing electrochemical testing on the anode material to be tested, and a target voltage parameter range capable of providing a judging basis for consistency is obtained from any one group of testing parameter sets. And obtaining a second target parameter according to the first target parameter in the target voltage parameter range, and obtaining a judgment parameter according to a plurality of second target parameters, so as to determine the consistency of the anode material to be detected according to the comparison result of the judgment parameter and the reference parameter. Therefore, the electrode material consistency determination method provided by the embodiment of the application avoids detecting multiple parameter indexes of the anode material to be detected, and only needs to extract target parameters (including a first target parameter and a second target parameter) from a test parameter group corresponding to an electrochemical test to obtain the determination parameters. Therefore, the electrode material consistency determination method provided by the embodiment of the application improves consistency determination efficiency.
Referring to fig. 3, in some embodiments, step S110 includes, but is not limited to, the substeps of:
s310, performing CV test or LSV test according to a preset scanning speed to obtain a plurality of candidate current parameters and a plurality of candidate voltage parameters;
s320, obtaining a group of test parameter sets according to the candidate current parameters and the candidate voltage parameters;
s330, adjusting the scanning speed, and executing the step S310 again to obtain a plurality of groups of test parameter sets.
Specifically, a three-electrode electrochemical system or a two-electrode electrochemical system is prepared according to the anode material to be detected, wherein the three-electrode electrochemical system comprises a working electrode, a reference electrode and an auxiliary electrode; the two-electrode electrochemical system comprises a working electrode and an auxiliary electrode. The negative electrode material to be detected comprises a negative electrode material used in a lithium ion battery, a sodium ion battery, a magnesium ion battery, an aluminum ion battery, a super capacitor and a pseudo capacitor, namely the negative electrode material to be detected comprises any one or more of MCMB (mesocarbon microbeads), soft carbon, hard carbon, graphite oxide, sulfonated graphite, graphene oxide, sulfonated graphene, carbon nanotubes, silicon oxide, a simple metal substance, a metal oxide, a metal sulfide, a titanium oxide, titanate and a titanium sulfide. The auxiliary electrode comprises any one of metal platinum, gold, palladium, lithium, sodium, magnesium and aluminum. The reference electrode comprises any one of metal platinum, gold, palladium, lithium, sodium, magnesium, aluminum, lithium iron phosphate, lithium titanate, calomel electrode, silver-silver chloride electrode, tribute-oxidation tribute electrode and hydrogen electrode.
Taking a two-electrode electrochemical system as an example, the negative electrode material to be tested is made into a working electrode, for example: selecting graphite asThe working electrode and the metal lithium are used as auxiliary electrodes, and LiPF is selected as electrolyte6And a diaphragm was Celgard2300, thereby preparing a test device. The test device is powered on, and is scanned at a preset scanning speed (i.e., a test condition), so as to obtain a plurality of candidate current parameters and a plurality of candidate voltage parameters corresponding to the scanning operation, thereby obtaining a set of test parameter sets corresponding to the scanning speed. And adjusting the scanning speed, and repeating the operation according to a plurality of different scanning speeds to obtain a plurality of groups of test parameter sets. It is understood that the scanning speed may be any value from 0.1mV/s to 100 mV/s.
For example, four sets of test parameter sets could be obtained according to the method described above, with scan speeds including 0.1mV/s, 0.5mV/s, 1.0mV/s, and 2.0 mV/s. And carrying out the cycle of oxidation reaction and reduction reaction at each scanning speed, and carrying out electrochemical test on the anode material to be tested from a low scanning speed to a high scanning speed until all the set scanning speeds are tested.
Secondly, to avoid side reactions during the scanning process and unnecessary time consumption, the voltage range of the CV test is limited to 0.01V to 3.00V, i.e., the candidate voltage parameter is between 0.01V and 3.00V.
In some embodiments, the test parameter set includes a first candidate parameter range representing an oxidation peak range, a second candidate parameter range representing a reduction peak range, and a third candidate parameter range representing a non-oxidation peak range, a non-reduction peak range. The step S120 "determining the target voltage parameter range from any one of the sets of test parameters" includes, but is not limited to, the following sub-steps:
and taking the third candidate parameter range of any one group of test parameter groups as the target voltage parameter range.
Specifically, CV test is taken as an example. CV curves are constructed for each of the plurality of sets of test parameters obtained by the above method, for example, referring to FIG. 2, a CV curve corresponding to a scanning speed of 0.5mV/s is taken as an example. In the CV test, when the triangular wave voltage (i.e., the candidate voltage parameter) increases (i.e., when the potential scans in the cathode direction), the electroactive substance is reduced on the working electrode, so as to obtain a reduction wave in the CV curve (as shown in fig. 2, 100); when the triangular wave voltage is reduced (i.e., the potential is swept toward the anode), the reduction product is oxidized again at the working electrode, and an oxidation wave (200 in fig. 2) in the CV curve is obtained. Thus, the CV curve may be divided into a reduction peak range, an oxidation peak range, and remaining ranges, wherein the oxidation peak range corresponds to a first candidate parameter range, the reduction peak range corresponds to a second candidate parameter range, and the remaining ranges correspond to a third candidate parameter range.
When the negative electrode material to be detected changes, namely the negative electrode material to be detected is inconsistent with the reference negative electrode material, the characteristic signal area of the non-Faraday capacitance in the CV curve is correspondingly changed, and the characteristic signal area of the non-Faraday capacitance corresponds to the third candidate parameter range. Therefore, the third candidate parameter range is used as the target voltage parameter range, that is, at least one candidate voltage parameter in the third candidate parameter range is processed, so that the judgment parameter for representing the current consistency of the anode material to be detected can be obtained.
Referring to fig. 4, in some embodiments, step S140 includes, but is not limited to, the substeps of:
s410, acquiring a scanning speed corresponding to the second target parameter;
and S420, in the same scanning direction, calculating to obtain a judgment parameter according to the plurality of second target parameters and the corresponding scanning speed.
Specifically, in the CV curve shown in fig. 2, the target voltage parameter range is a candidate voltage parameter corresponding to 1.2V to 3.0V. And selecting one candidate voltage parameter from the target voltage parameter range as a first target parameter, such as 2.5V. And respectively searching candidate current parameters corresponding to 2.5V in the four groups of test parameter sets, and taking the candidate current parameters obtained by searching as second target parameters so as to obtain four second target parameters.
It is understood that the characteristic signal region of the non-faradaic capacitor can be expressed as the relation: I/Vscan is K1, where I represents a candidate current parameter, Vscan represents a scanning speed, and K1 represents a slope (i.e., a determination parameter). Therefore, in the same scanning direction, a current-scanning speed map is constructed according to the four second target parameters and the scanning speeds corresponding to the four second target parameters (as shown in fig. 5). The same scanning direction includes any one of an increasing direction of the candidate voltage parameter and a decreasing direction of the candidate voltage parameter, that is, any one of a potential scanning in a cathode direction and a potential scanning in an anode direction. Referring to fig. 5, taking the same scanning direction as the candidate voltage parameter increasing direction as an example, a candidate current parameter-scanning speed map is constructed according to the candidate current parameters corresponding to 2.5V at the scanning speeds of 0.1mV/s, 0.5mV/s, 1.0mV/s and 2.0mV/s, and a slope value K1 corresponding to the candidate current parameter-scanning speed map is calculated, thereby obtaining the determination parameter.
Referring to fig. 6, in some embodiments, step S150 includes, but is not limited to, the substeps of:
s610, if the comparison result shows that the judgment parameter is equal to the reference parameter, judging that the consistency of the negative electrode material to be detected is a first level;
and S620, if the comparison result shows that the judgment parameter is not equal to the reference parameter, judging that the consistency of the to-be-detected anode material is of a second level.
Specifically, the judgment parameters are compared with the reference parameters, if the comparison result shows that the judgment parameters are not equal, the judgment result shows that at least one of the particle size distribution, the specific surface area, the tap density, the morphology, the crystal structure and the like of the anode material to be detected is different from the reference anode material, and at the moment, the consistency of the anode material to be detected is judged to be a first level; if the comparison results show that the particle size distribution, the specific surface area, the tap density, the morphology, the crystal structure and the like of the negative electrode material to be detected are equal to those of the reference negative electrode material, the consistency of the negative electrode material to be detected is judged to be the second level, and therefore the qualitative judgment of the consistency of the negative electrode material to be detected is achieved.
Referring to FIG. 7, in other embodiments, step S150 includes, but is not limited to, the substeps of:
s710, if the comparison result shows that the judgment parameter is not equal to the reference parameter, acquiring a difference value between the judgment parameter and the reference parameter;
and S720, if the difference value is within a preset range, judging that the consistency of the negative electrode material to be detected is a preset grade corresponding to the preset range.
Specifically, a plurality of preset ranges are preset, and each preset range corresponds to one preset level. When the judgment parameter is determined to be unequal to the reference parameter, the difference value between the judgment parameter and the reference parameter is obtained, and the preset range containing the difference value is searched, so that the consistency of the anode material to be detected is determined according to the preset grade corresponding to the preset range, and the quantitative judgment of the consistency of the anode material to be detected is further realized. It is to be understood that the difference value includes any one of a difference value, a change rate, and the like, and the embodiment of the present application is not particularly limited.
Hereinafter, taking different types of negative electrode materials to be measured as examples, the quantitative determination of the consistency of the negative electrode materials to be measured will be specifically described.
Firstly, in some embodiments, graphite is selected as a negative electrode material to be detected, the negative electrode material to be detected is used as a working electrode, an auxiliary electrode is selected from metal lithium, an electrolyte is selected from LiPF6, a diaphragm is selected from Celgard2300, and a two-electrode electrochemical system to be detected is formed according to the working electrode, the auxiliary electrode, the electrolyte and the diaphragm in an assembling manner. Four scanning speeds of 0.1mV/s, 0.5mV/s, 1.0mV/s and 2.0mV/s are set, and the determination parameters of the anode material to be tested are calculated according to the method described in any one of the above embodiments.
Table 1:
| slope value K2 | Rate of change | Preset grade | |
| Reference negative electrode material | 1.64E-04 | 0.0％ | / |
Table 2:
| negative electrode material to be measured | Slope value K1 | Rate of change | Preset grade |
| Particle size D50 reduction of 1um | 1.42E-04 | -13.2％ | In |
| Particle size D50 increased by 1.5um | 2.06E-04 | 25.7％ | Difference (D) |
| Increase in particle diameter D50 by 3um | 2.43E-04 | 48.0％ | Difference (D) |
| The graphitization degree is reduced by 1 percent | 1.50E-04 | -8.7％ | Good taste |
| The graphitization degree is increased by 1 percent | 1.75E-04 | 6.5％ | Good taste |
| The graphitization degree is increased by 2 percent | 1.94E-04 | 18.1％ | In |
| The specific surface area is reduced by 20 percent | 2.08E-04 | 27.1％ | Difference between |
| The specific surface area is reduced by 10 percent | 1.95E-04 | 18.8％ | In |
| The specific surface area is increased by 10 percent | 1.85E-04 | 12.9％ | In |
| The tap density is reduced by 15 percent | 1.86E-04 | 13.5％ | In |
| The tap density is increased by 15 percent | 1.96E-04 | 19.4％ | In |
Referring to tables 1 and 2, taking the example where the change rate indicates the difference value, three preset ranges of 0. ltoreq. x < 10%, 10. ltoreq. x < 20%, and x. ltoreq.20% are preset, where x indicates the absolute value of the change rate, 0. ltoreq. x < 10% indicates that the preset rank is "good", 10. ltoreq. x < 20% indicates that the preset rank is "medium", and x. ltoreq.20% indicates that the preset rank is "poor". It can be understood that, corresponding to the two-electrode electrochemical system to be measured, the reference two-electrode electrochemical system uses the reference negative electrode material as the working electrode, and the components of each part in the reference two-electrode electrochemical system are equal to those of the two-electrode electrochemical system to be measured, i.e. the auxiliary electrode of the reference two-electrode electrochemical system is made of metal lithium, and the electrolyte is made of LiPF6The diaphragm is Celgard 2300. The slope value K2 (i.e., the baseline parameter) of the baseline negative electrode material was calculated to be 1.64E-04 according to the method described in any of the above examples.
As shown in table 2, when the particle diameter D50 of the anode material to be measured is reduced by 1 μm compared with the particle diameter D50 of the reference anode material, the slope value K1 (i.e., the determination parameter) of the anode material to be measured is 1.42E-04, and the change rate of the determination parameter is-13.2% compared with the reference parameter, and then the consistency of the anode material to be measured is determined to be medium. When the particle diameter D50 of the negative electrode material to be measured is increased by 1.5 μm compared with the particle diameter D50 of the reference negative electrode material, the slope value K1 of the negative electrode material to be measured is 2.06E-04, the change rate of the determination parameter compared with the reference parameter is 25.7%, and the consistency of the negative electrode material to be measured is determined to be poor. When the particle diameter D50 of the negative electrode material to be measured is increased by 3 μm compared with the particle diameter D50 of the reference negative electrode material, the slope value K1 of the negative electrode material to be measured is 2.43E-04, the change rate of the determination parameter compared with the reference parameter is 48.0%, and the consistency of the negative electrode material to be measured is determined to be poor. It can be understood that when the graphitization degree, the specific surface area, and the array density of the negative electrode material to be detected change, the preset grade corresponding to the negative electrode material to be detected can be obtained by referring to table 2, and details are not repeated for the embodiment of the present application.
In other embodiments, a composite of graphene and iron oxide is selected as a negative electrode material to be detected, the negative electrode material to be detected is used as a working electrode, an auxiliary electrode is made of metal platinum, an electrolyte is selected from a 1.0M potassium hydroxide standard titration solution, a mercury-mercury oxide electrode is selected as a reference electrode, and a three-electrode electrochemical system to be detected is formed by assembling the working electrode, the auxiliary electrode, the electrolyte and the reference electrode. Taking the LSV test as an example, four scanning speeds of 0.01mV/s, 1.0mV/s, 10mV/s and 100mV/s are set, and according to the method described in any of the above embodiments, the candidate voltage parameter decreasing direction is taken as the same scanning direction, and the determination parameter of the anode material to be tested is calculated.
Table 3:
| slope value K2 | Rate of change | Preset grade | |
| Reference negative electrode material | 2.71E-02 | 0.0％ | / |
Table 4:
referring to tables 3 and 4, taking the example where the change rate indicates the difference value, three preset ranges of 0. ltoreq. x < 10%, 10. ltoreq. x < 20%, and x. ltoreq.20% are preset, where x indicates the absolute value of the change rate, 0. ltoreq. x < 10% indicates that the preset rank is "good", 10. ltoreq. x < 20% indicates that the preset rank is "medium", and x. ltoreq.20% indicates that the preset rank is "poor". It can be understood that, corresponding to the three-electrode electrochemical system to be measured, the reference three-electrode electrochemical system uses the reference negative electrode material as the working electrode, and the components of each part in the reference three-electrode electrochemical system are equal to those of the three-electrode electrochemical system to be measured. The slope value K2 (i.e., the reference parameter) of the reference anode material was calculated to be 2.71E-02 according to the method described in any of the above examples.
As shown in table 4, when the iron oxide proportion of the negative electrode material to be measured is increased by 1 wt.% compared with the iron oxide proportion of the reference negative electrode material, the slope value K1 (i.e., the determination parameter) of the negative electrode material to be measured is 3.04E-02, the change rate of the determination parameter compared with the reference parameter is 12.2%, and the consistency of the negative electrode material to be measured is determined to be medium. When the iron oxide proportion of the negative electrode material to be detected is reduced by 5 wt.% compared with that of the reference negative electrode material, the slope value K1 of the negative electrode material to be detected is 1.98E-02, the change rate of the determination parameter compared with the reference parameter is-26.8%, and the consistency of the negative electrode material to be detected is determined to be poor. It can be understood that when the particle size of the iron oxide of the negative electrode material to be detected changes, the preset grade corresponding to the negative electrode material to be detected can be obtained by referring to table 4, and details of the embodiment of the present application are not repeated.
Finally, in other embodiments, molybdenum disulfide is selected as a negative electrode material to be detected, the negative electrode material to be detected is used as a working electrode, an auxiliary electrode is selected from magnesium metal, an electrolyte is selected from 0.5M Mg (BH4)2 (the volume ratio of DME to THF is 1: 1), a diaphragm is selected from Celgard2300, and a two-electrode electrochemical system to be detected is formed by assembling the working electrode, the auxiliary electrode, the electrolyte and the diaphragm. And setting four scanning speeds of 0.1mV/s, 0.5mV/s, 5.0mV/s and 50mV/s, and calculating the judgment parameter of the anode material to be tested according to the method described in any one of the above embodiments.
Table 5:
| slope value K2 | Rate of change | Preset grade | |
| Reference negative electrode material | 9.30E-04 | 0.0％ | / |
Table 6:
| negative electrode material to be measured | Slope value K1 | Rate of change | Preset grade |
| The specific surface area is increased by 10 percent | 1.11E-03 | 19.2％ | In |
| The specific surface area is reduced by 5 percent | 8.31E-04 | -10.6％ | In |
| The tap density is increased by 20 percent | 4.67E-04 | -49.8％ | Difference (D) |
| The tap density is reduced by 10 percent | 1.09E-03 | 17.7％ | In |
Referring to tables 5 and 6, taking the example where the change rate indicates the difference value, three preset ranges of 0. ltoreq. x < 10%, 10. ltoreq. x < 20%, and x. ltoreq.20% are preset, where x indicates the absolute value of the change rate, 0. ltoreq. x < 10% indicates that the preset rank is "good", 10. ltoreq. x < 20% indicates that the preset rank is "medium", and x. ltoreq.20% indicates that the preset rank is "poor". It can be understood that, corresponding to the two-electrode electrochemical system to be measured, the reference two-electrode electrochemical system uses the reference negative electrode material as the working electrode, and the components of each part in the reference two-electrode electrochemical system are equal to those of the two-electrode electrochemical system to be measured. The slope value K2 (i.e., the reference parameter) of the reference anode material calculated according to the method described in any of the above examples was 9.30E-04.
As shown in table 6, when the specific surface area of the anode material to be measured is increased by 10% compared with the specific surface area of the reference anode material, the slope value K2 (i.e., the determination parameter) of the anode material to be measured is 1.11E-03, and the change rate of the determination parameter compared with the reference parameter is 19.2%, at which time the consistency of the anode material to be measured is determined to be medium. When the specific surface area of the negative electrode material to be detected is reduced by 5% compared with that of the reference negative electrode material, the slope value K2 of the negative electrode material to be detected is 8.31E-04, the change rate of the judgment parameter is-10.6% compared with that of the reference parameter, and the consistency of the negative electrode material to be detected is judged to be middle. It can be understood that when the specific surface area and the tap density of the negative electrode material to be detected change, the preset grade corresponding to the negative electrode material to be detected can be obtained by referring to table 6, and details of the embodiment of the present application are not repeated.
According to the electrode material consistency determination method provided by the embodiment of the application, electrochemical testing is performed on the negative electrode material to be determined, and the third candidate parameter range corresponding to the non-Faraday capacitance characteristic signal area in the testing parameter group is selected as the target voltage parameter range, so that the determination parameter capable of representing the consistency change of the negative electrode material to be determined is obtained according to the target voltage parameter range, and then qualitative determination and/or quantitative determination of the consistency of the negative electrode material to be determined is realized according to the comparison result of the determination parameter and the reference parameter. Therefore, the judgment method provided by the embodiment of the application avoids testing multiple parameter indexes of the negative electrode material to be tested, and improves the judgment efficiency of the consistency of the negative electrode material to be tested.
Referring to fig. 8, an embodiment of the present application further provides an electrode material consistency determination system. The determination system includes:
the testing module 801 is used for performing multiple electrochemical tests on the negative electrode material to obtain multiple groups of testing parameter sets; wherein the electrochemical test comprises a CV test or an LSV test; each group of test parameter group comprises a plurality of candidate current parameters and candidate voltage parameters corresponding to the candidate current parameters;
a first query module 802, configured to determine a target voltage parameter range from any one of the sets of test parameters, and use at least one candidate voltage parameter in the target voltage parameter range as a first target parameter;
a second query module 803, configured to obtain a candidate current parameter corresponding to the first target parameter from the multiple sets of test parameters, and use the candidate current parameter as a second target parameter;
a calculating module 804, configured to calculate a decision parameter according to the plurality of second target parameters;
the determining module 805 is configured to compare the determining parameter with a preset reference parameter, and determine consistency of the negative electrode material to be detected according to a comparison result.
Secondly, the judging system also comprises a testing device which is a three-electrode electrochemical system or a two-electrode electrochemical system. The preparation material of the working electrode of the testing device is a material to be tested, and the testing module 801 is used for performing multiple electrochemical tests on the testing device.
It can be seen that the contents in the above embodiments of the electrode material consistency determination method are all applicable to the embodiments of the present electrode material consistency determination system, and the functions specifically implemented by the embodiments of the present electrode material consistency determination system are the same as those of the above embodiments of the electrode material consistency determination method, and the beneficial effects achieved by the embodiments of the present electrode material consistency determination method are also the same as those achieved by the above embodiments of the electrode material consistency determination method.
An embodiment of the present application further provides an electronic device, including: the system includes at least one processor, and a memory communicatively coupled to the at least one processor. The memory stores instructions, and the instructions are executed by the at least one processor, so that the at least one processor can implement the electrode material consistency determination method as described in any one of the above embodiments when executing the instructions.
An embodiment of the present application provides a computer-readable storage medium storing computer-executable instructions for: the electrode material consistency determination method described in any of the above embodiments is performed.
The above-described embodiments of the apparatus are merely illustrative, wherein the units illustrated as separate components may or may not be physically separate, i.e. may be located in one place, or may also be distributed over a plurality of network elements. Some or all of the modules may be selected according to actual needs to achieve the purpose of the solution of the present embodiment.
One of ordinary skill in the art will appreciate that all or some of the steps, systems, and methods disclosed above may be implemented as software, firmware, hardware, and suitable combinations thereof. Some or all of the physical components may be implemented as software executed by a processor, such as a central processing unit, digital signal processor, or microprocessor, or as hardware, or as an integrated circuit, such as an application specific integrated circuit. Such software may be distributed on computer readable media, which may include computer storage media (or non-transitory media) and communication media (or transitory media). The term computer storage media includes volatile and nonvolatile, removable and non-removable media implemented in any method or technology for storage of information such as computer readable instructions, data structures, program modules or other data, as is well known to those of ordinary skill in the art. Computer storage media includes, but is not limited to, RAM, ROM, EEPROM, flash memory or other memory technology, CD-ROM, Digital Versatile Disks (DVD) or other optical disk storage, magnetic cassettes, magnetic tape, magnetic disk storage or other magnetic storage devices, or any other medium which can be used to store the desired information and which can accessed by a computer. In addition, communication media typically embodies computer readable instructions, data structures, program modules or other data in a modulated data signal such as a carrier wave or other transport mechanism and includes any information delivery media as known to those skilled in the art.
The embodiments of the present application have been described in detail with reference to the drawings, but the present application is not limited to the embodiments, and various changes can be made within the knowledge of those skilled in the art without departing from the gist of the present application. Furthermore, the embodiments and features of the embodiments of the present application may be combined with each other without conflict.
Claims (10)
1. The electrode material consistency determination method is characterized by comprising the following steps:
carrying out multiple electrochemical tests on the material to be tested to obtain multiple groups of test parameter sets; wherein the electrochemical test comprises a CV test or an LSV test; each group of the test parameter sets comprises a plurality of candidate current parameters and candidate voltage parameters corresponding to the candidate current parameters;
determining a target voltage parameter range from any one group of test parameter sets, and taking at least one candidate voltage parameter in the target voltage parameter range as a first target parameter;
obtaining the candidate current parameter corresponding to the first target parameter from a plurality of groups of the test parameter sets, and taking the candidate current parameter as a second target parameter;
calculating according to the plurality of second target parameters to obtain a judgment parameter;
and comparing the judgment parameters with preset reference parameters, and judging the consistency of the material to be detected according to the comparison result.
2. The electrode material consistency determination method according to claim 1, wherein the test parameter group includes candidate parameter ranges representing a non-oxidation peak range and a non-reduction peak range;
the determining a target voltage parameter range from any one set of the test parameter sets comprises:
and taking the candidate parameter range of any one group of the test parameter groups as the target voltage parameter range.
3. The method for determining the consistency of an electrode material according to claim 1, wherein the step of performing a plurality of electrochemical tests on the material to be tested to obtain a plurality of test parameter sets comprises:
performing CV test or LSV test according to a preset scanning speed to obtain a plurality of candidate current parameters and a plurality of candidate voltage parameters;
obtaining a group of test parameter sets according to the candidate current parameters and the candidate voltage parameters;
and adjusting the scanning speed, and executing the scanning operation according to the preset scanning speed again to obtain a plurality of groups of test parameter sets.
4. The electrode material consistency determination method according to claim 3, wherein the calculating a determination parameter from a plurality of second target parameters includes:
acquiring the scanning speed corresponding to the second target parameter;
in the same scanning direction, calculating to obtain the judgment parameter according to the plurality of second target parameters and the corresponding scanning speed;
wherein the same scanning direction includes any one of the candidate voltage parameter increasing direction and the candidate voltage parameter decreasing direction.
5. The electrode material consistency determination method according to any one of claims 1 to 4, wherein the determining the consistency of the material to be measured based on the comparison result includes:
if the comparison result shows that the judgment parameter is equal to the reference parameter, judging that the consistency of the material to be detected is a first level;
and if the comparison result shows that the judgment parameter is not equal to the reference parameter, judging that the consistency of the material to be detected is a second level.
6. The electrode material consistency determination method according to any one of claims 1 to 4, wherein the determining the consistency of the material to be measured based on the comparison result includes:
if the comparison result shows that the judgment parameter is not equal to the reference parameter, acquiring a difference value between the judgment parameter and the reference parameter;
and if the difference value is within a preset range, judging that the consistency of the material to be detected is a preset grade corresponding to the preset range.
7. An electrode material consistency determination system, comprising:
the test module is used for carrying out multiple electrochemical tests on the material to be tested to obtain multiple groups of test parameter sets; wherein the electrochemical test comprises a CV test or an LSV test; each group of the test parameter sets comprises a plurality of candidate current parameters and candidate voltage parameters corresponding to the candidate current parameters;
a first query module, configured to determine a target voltage parameter range from any one of the sets of test parameters, and use at least one candidate voltage parameter in the target voltage parameter range as a first target parameter;
the second query module is used for obtaining the candidate current parameter corresponding to the first target parameter from a plurality of groups of test parameter sets and taking the candidate current parameter as a second target parameter;
the calculation module is used for calculating to obtain a judgment parameter according to the plurality of second target parameters;
and the judging module is used for comparing the judging parameters with preset reference parameters and judging the consistency of the material to be detected according to the comparison result.
8. The electrode material consistency determination system according to claim 7, characterized by further comprising:
the device comprises a testing device, a detection device and a control device, wherein the testing device is a three-electrode electrochemical system or a two-electrode electrochemical system;
the preparation material of the working electrode of the testing device is the material to be tested; the test module is used for carrying out the electrochemical test on the test device for a plurality of times.
9. An electronic device, comprising:
at least one processor;
at least one memory for storing at least one program;
when the at least one program is executed by the at least one processor, causing the at least one processor to implement the electrode material consistency determination method according to any one of claims 1 to 6.
10. A computer-readable storage medium having stored therein processor-executable instructions, wherein the processor-executable instructions, when executed by a processor, are for implementing the electrode material consistency determination method of any one of claims 1 to 6.
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| CN116027138B (en) * | 2023-03-28 | 2023-08-25 | 南通江海储能技术有限公司 | Consistency test method and system for super capacitor |
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