CN111505520A - Method and system for rapidly verifying corrosion behavior of lead-acid storage battery - Google Patents
Method and system for rapidly verifying corrosion behavior of lead-acid storage battery Download PDFInfo
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- G01R31/36—Arrangements for testing, measuring or monitoring the electrical condition of accumulators or electric batteries, e.g. capacity or state of charge [SoC]
- G01R31/392—Determining battery ageing or deterioration, e.g. state of health
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- G—PHYSICS
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- G01R—MEASURING ELECTRIC VARIABLES; MEASURING MAGNETIC VARIABLES
- G01R31/00—Arrangements for testing electric properties; Arrangements for locating electric faults; Arrangements for electrical testing characterised by what is being tested not provided for elsewhere
- G01R31/36—Arrangements for testing, measuring or monitoring the electrical condition of accumulators or electric batteries, e.g. capacity or state of charge [SoC]
- G01R31/378—Arrangements for testing, measuring or monitoring the electrical condition of accumulators or electric batteries, e.g. capacity or state of charge [SoC] specially adapted for the type of battery or accumulator
- G01R31/379—Arrangements for testing, measuring or monitoring the electrical condition of accumulators or electric batteries, e.g. capacity or state of charge [SoC] specially adapted for the type of battery or accumulator for lead-acid batteries
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- G01R31/00—Arrangements for testing electric properties; Arrangements for locating electric faults; Arrangements for electrical testing characterised by what is being tested not provided for elsewhere
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Abstract
The invention discloses a method and a system for rapidly verifying corrosion behavior of a lead-acid storage battery, wherein the method comprises the following steps: the method comprises the following steps: after positive and negative plates are respectively coated by diaphragms and combined into a plate group, the plate group to be tested is respectively placed in electrolytes with different concentrations for charging test, and the potential change condition and the charging quantity of the positive electrode in the charging process are recorded; step two: soaking the charged positive plate in pure water, cleaning and drying, and detecting the thickness of the grid corrosion layer of the positive plate; step three: and (4) placing the positive plate with the corrosion layer after the charging in the step one in electrolyte with the same concentration, and testing the conductivity of the corrosion layer at the interface of the positive plate. By manufacturing the positive and negative plates for verification, the subsequent processes of battery assembly, welding and the like are saved, the verification period of corrosion behavior can be shortened, and the cost of raw materials is saved.
Description
Technical Field
The invention belongs to the field of lead-acid storage battery performance verification, and particularly relates to a method and a system for rapidly verifying corrosion behavior of a lead-acid storage battery.
Background
The lead-acid storage battery is used as the earliest secondary battery, and is widely applied to the fields of energy storage, communication, start and stop and the like due to the advantages of mature technology, safety, stability, low price and the like. However, due to the impact of new energy batteries such as lithium ion batteries and the relatively short cycle life of the batteries, the market share of the batteries is gradually reduced, and the competitiveness of the batteries is also gradually reduced. Therefore, the main problem to be solved at the present stage is how to improve the performance of the lead-acid storage battery.
The corrosion of the positive grid is an important factor causing the failure of the lead-acid storage battery, so the method plays an important role in verifying the corrosion behavior of the lead-acid storage battery and prolonging the service life of the battery. The positive electrode is extremely easy to corrode under the condition of high potential for a long time, and the potential influences the corrosion of a positive electrode grid and the electrolyte density influences the potential according to the kinetic principle, so that the method has a certain guiding effect on the verification of the electrolyte concentration and the improvement of the service life of the battery.
Disclosure of Invention
The invention aims to provide a method and a system for rapidly verifying the corrosion behavior of a lead-acid storage battery, which are used for overcoming the defects in the prior art.
The invention is realized by the following technical scheme:
a method for rapidly verifying the corrosion behavior of a lead-acid storage battery comprises the following steps:
the method comprises the following steps: after positive and negative plates are respectively coated by diaphragms and combined into a plate group, the plate group to be tested is respectively placed in electrolytes with different concentrations for charging test, and the potential change condition and the charging quantity of the positive electrode in the charging process are recorded;
step two: soaking the charged positive plate in pure water, cleaning and drying, and detecting the thickness of the grid corrosion layer of the positive plate;
step three: and (4) placing the positive plate with the corrosion layer after the charging in the step one in electrolyte with the same concentration, and testing the conductivity of the corrosion layer at the interface of the positive plate.
According to the method for rapidly verifying the corrosion behavior of the lead-acid storage battery, in the first step, the positive plate can be adjusted in different alloy proportions according to verification requirements.
According to the method for rapidly verifying the corrosion behavior of the lead-acid storage battery, the electrolyte selected in the first step is H2SO4And (3) an electrolyte.
In the method for rapidly verifying the corrosion behavior of the lead-acid storage battery, in the first step, the charging mode of the positive plate is a constant-voltage current-limiting charging mode.
The method for rapidly verifying the corrosion behavior of the lead-acid storage battery is described as above, and the charging operation in the first step is as follows: positive and negative electrode plates, Hg/Hg2SO4The electrodes are respectively used as a working electrode, a counter electrode and a reference electrode to be connected with the electrochemical workstation, meanwhile, the positive plate and the negative plate are also respectively connected with the positive electrode and the negative electrode of the charging motor, and the measurement of the potential of the positive electrode and the measurement of the charging quantity in the charging process can be accurately known through a computer connected with the electrochemical workstation.
In the second step, the positive plate is soaked in pure water, cleaned, dried, and then frozen and stored on the surface of the positive plate, and then sent to be subjected to grid corrosion layer thickness detection.
In the method for rapidly verifying the corrosion behavior of the lead-acid storage battery, in the second step, the positive plate is soaked in pure water, washed, dried and then placed in liquid nitrogen for freezing to obtain a plate to be tested, and the thickness of the grid corrosion layer of the plate is tested by adopting SEM.
The method for rapidly verifying the corrosion behavior of the lead-acid storage battery comprises the following specific operations of testing the conductivity of the corrosion layer at the interface of the positive plate in the third step: the positive plate is used as a working electrode, the large-area graphite plate is used as a counter electrode, and Hg/Hg is2SO4The positive plate and the large-area graphite plate are respectively connected with the positive electrode and the negative electrode of the charging motor, and the conduction condition of the corrosion layer on the interface of the positive plate is tested.
According to the method for rapidly verifying the corrosion behavior of the lead-acid storage battery, the electrolyte selected in the third step is H2SO4And (3) an electrolyte.
A system for rapidly verifying corrosion behavior of a lead-acid battery, comprising: the device comprises a positive plate, a negative plate, a battery jar, an electrochemical workstation and a charging motor;
the positive plate and the negative plate are respectively coated by a diaphragm and combined into a plate group; the pole group is arranged in the electrolyte of the battery jar;
positive and negative plates and Hg/Hg2SO4The electrodes are respectively used as a working electrode, a counter electrode and a reference electrode to be connected with an electrochemical workstation, and meanwhile, the positive plate and the negative plate are respectively connected with the positive pole and the negative pole of the charging motor.
Compared with the prior art, the invention has the following advantages:
1. by manufacturing the positive and negative plates for verification, the subsequent processes of battery assembly, welding and the like are saved, the verification period of corrosion behavior can be shortened, and the cost of raw materials is saved;
2. through verification of corrosion behaviors of the positive plate in electrolytes with different concentrations, the aim of optimizing the concentration of the electrolyte in the formation process can be achieved.
3. By testing the alternating current impedance of the positive plate after corrosion, the conductivity and the charge conduction capability of the interface corrosion layer can be determined, the corrosion behavior can be rapidly verified, and data support is provided for the preferable alloy material and the lead paste formula.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings needed to be used in the description of the embodiments or the prior art will be briefly introduced below, and it is obvious that the drawings in the following description are some embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to these drawings without creative efforts.
FIG. 1 is a schematic diagram of a test structure of the present invention;
FIG. 2 is a broken line diagram showing the results of potential measurements at the end of charge of the positive electrode plate in examples 1 to 4;
fig. 3 is a positive plate ac impedance test curve for examples 1-4.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are some, but not all, embodiments of the present invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Referring to fig. 1, the present invention provides a system for rapidly verifying corrosion behavior of a lead-acid battery, comprising: a positive plate 1, a negative plate 2, a battery jar 10, an electrochemical workstation 11 and a charging motor 21;
the positive plate 1 and the negative plate 2 are respectively coated by a diaphragm 3 and combined into a plate group; the pole group is arranged in the electrolyte 4 of the battery jar 10;
positive and negative plates 1 and 2 and Hg/Hg2SO4The electrodes are respectively used as a working electrode, a counter electrode and a reference electrode to be connected with an electrochemical workstation 11, and meanwhile, the positive plate 1 and the negative plate 2 are respectively connected with a positive electrode 8 and a negative electrode 9 of a charging motor 21.
The invention provides a method for rapidly verifying corrosion behavior of a lead-acid storage battery, which comprises the following steps:
the method comprises the following steps: after the positive plate 1 and the negative plate 2 are respectively coated by the diaphragm 3 and combined into a plate group, the plate group to be tested is respectively placed in the electrolyte 4 of the battery jar 10 with different concentrations for charging test, and the change situation of the positive electrode potential and the charged electric quantity in the charging process are recorded;
step two: soaking the charged positive plate 1 in pure water, cleaning and drying, and detecting the thickness of the grid corrosion layer of the positive plate 1;
step three: and (3) placing the positive plate 1 with the corrosion layer after the charging in the step one in the electrolyte with the same concentration, and testing the conductivity of the corrosion layer at the interface of the positive plate.
The charging operation in the first step is as follows: positive plate 1, negative plate 2, Hg/Hg2SO4The electrodes are respectively used as a working electrode 7, a counter electrode 6 and a reference electrode 5 to be connected with an electrochemical workstation 11, meanwhile, the positive plate 1 and the negative plate 2 are also respectively connected with a positive electrode 8 and a negative electrode 9 of a charging motor 21, and the measurement of the potential of the positive electrode and the measurement of the charging quantity in the charging process can be accurately known through a computer connected with the electrochemical workstation.
Example 1
Preparing positive plate grid from Pb-Ca-Sn-Al alloy, preparing positive plate, coating negative plate and prepared positive plate with diaphragm, combining them to obtain electrode group, and placing the electrode group in 1.290g/cm3H of (A) to (B)2SO4In the electrolyte, a charge-discharge machine is connected to perform a constant-voltage 2.35V current-limiting 0.1C charging 24h charging test, an electrochemical workstation is adopted, and a positive plate, a negative plate and Hg/Hg are respectively adopted2SO4The electrode is a working electrode, a counter electrode and a reference electrode, and the potential of the positive electrode and the charging quantity in the charging process are measured.
Example 2
Preparing positive plate grid from Pb-Ca-Sn-Al alloy, preparing positive plate, wrapping the negative plate and the prepared positive plate with diaphragm, combining them to obtain electrode group, and placing the electrode group in 1.320g/cm3H of (A) to (B)2SO4In the electrolyte, a charge-discharge machine is connected to perform a constant-voltage 2.35V current-limiting 0.1C charging 24h charging test, an electrochemical workstation is adopted, and a positive plate, a negative plate and Hg/Hg are respectively adopted2SO4The electrode is a working electrode, a counter electrode and a reference electrode, and the potential of the positive electrode and the charging quantity in the charging process are measured.
Example 3
Preparing positive plate grid from Pb-Ca-Sn-Al-Ba alloy, preparing positive plate, wrapping the negative plate and the prepared positive plate with diaphragm, combining them to form electrode group, and placing the electrode group in 1.290g/cm3H of (A) to (B)2SO4In the electrolyte, a charge-discharge machine is connected to perform a constant-voltage 2.35V current-limiting 0.1C charging 24h charging test, an electrochemical workstation is adopted, and a positive plate, a negative plate and Hg/Hg are respectively adopted2SO4The electrode is a working electrode, a counter electrode and a reference electrode, and is used in the charging processAnd measuring the potential of the anode and the charge quantity.
Example 4
Preparing positive plate grid from Pb-Ca-Sn-Al-Ba alloy, preparing positive plate, wrapping the negative plate and the prepared positive plate with diaphragm, combining them to form electrode group, and placing the electrode group in 1.320g/cm3H of (A) to (B)2SO4In the electrolyte, a charge-discharge machine is connected to perform a constant-voltage 2.35V current-limiting 0.1C charging 24h charging test, an electrochemical workstation is adopted, and a positive plate, a negative plate and Hg/Hg are respectively adopted2SO4The electrode is a working electrode, a counter electrode and a reference electrode, and the potential of the positive electrode and the charging quantity in the charging process are measured.
The results of the potential measurements at the last stage of charge of the positive electrode plates of examples 1 to 4 are shown in fig. 2, and the results of the measurements of the charge amount of the positive electrode plates are shown in table 1:
TABLE 1 Positive plate Charge
| Examples | Charge capacity (%) |
| Example 1 | 105.6 |
| Example 2 | 94.4 |
| Example 3 | 109.2 |
| Example 4 | 98.1 |
Verification test
First, measurement of thickness of corrosion layer
The positive electrode plates obtained in examples 1 to 4 were respectively immersed in pure water, washed, dried, and then subjected to freeze preservation of the surface of the positive electrode plate, and then subjected to a gate corrosion layer thickness test, and the test results are shown in table 2:
TABLE 2 thickness of corrosion layer under different electrolyte concentrations and alloy compositions of positive grid
| Examples | Thickness of positive grid corrosion layer (mum) |
| Example 1 | 30.2 |
| Example 2 | 35.8 |
| Example 3 | 25.6 |
| Example 4 | 32.3 |
Second, AC impedance test under different electrolyte concentrations and alloy compositions of positive plate
The positive plates with the corrosion layers obtained in examples 1 to 4 were placed at 1.300g/cm each3H of (A) to (B)2SO4In the electrolyte, an alternating current impedance test is carried out, wherein a positive plate is used as a working electrode, a large-area graphite plate is used as a counter electrode, and Hg/Hg is used2SO4As reference electrode, the three are respectively connected with electrochemical workstation, and positive plate and large-area graphite plate are respectively connected with positive electrode and negative electrode of charging motor at the same time, test example1-4, obtaining fitted data of the alternating current impedance test of the positive plate of the embodiment 1-4 under different electrolyte concentrations and alloy components, wherein the alternating current impedance test curve of the positive plate is shown in fig. 3; data results are shown in table 3:
TABLE 3 AC impedance test fitting data for different electrolyte concentrations and alloy compositions of positive plate
| Examples | Rs | R1 | Rct |
| Example 1 | 0.0340 | 0.0254 | 0.0942 |
| Example 2 | 0.0268 | 0.0292 | 0.1118 |
| Example 3 | 0.0370 | 0.0216 | 0.0699 |
| Example 4 | 0.0257 | 0.0282 | 0.0990 |
Wherein R issIs ohmic resistance, R1For etching the film resistance, RctIs a charge transfer resistor.
As can be seen from the data in table 1, the charging order of the positive electrode is example 3> example 1> example 4> example 2, which indicates that an increase in the electrolyte concentration may result in a decrease in the rate of electrochemical reaction during charging. As shown in fig. 2, the increase in the electrolyte concentration causes an increase in the potential at the last stage of positive electrode charging, which indicates that the increase in the electrolyte concentration promotes corrosion of the positive electrode grid, while the addition of Ba to the alloy causes a slight decrease in the potential at the last stage of positive electrode charging, which indicates that the addition of Ba suppresses corrosion of the positive electrode grid.
As can be seen from the data in table 2, the corrosion resistance of the positive grid is example 3> example 1> example 4> example 2.
As can be seen from the data in table 3, the corrosion film resistance and the charge transfer resistance of example 3 are the smallest, which indicates that the alloy composition and the test conditions of example 3 are the best for the conductivity and the interfacial charge conductivity of the corrosion layer of the positive grid of the lead-acid battery.
According to the corrosion behavior verification performed by the method, whether the electrolyte can cause corrosion failure of the positive grid or not can be judged through the corrosion layer thickness of the positive grid and the potential change condition in the charging process under the condition of electrolytes with different concentrations; according to the condition of the charged electric quantity in the charging process, whether the concentration of the electrolyte of the lead-acid storage battery is qualified or not and whether the passivation of the anode can be caused or not can be judged, so that the charging and discharging reaction is influenced, and the battery cannot be fully charged. And suitable electrolyte concentrations were sought for batteries of different positive electrode raw material formulations.
According to the alternating current impedance test of the positive plate, the conductivity and the charge conduction condition of the corrosion layer of the positive plate grid/active material interface can be rapidly judged, and a certain data supporting effect is realized on the screened alloy formula and the lead paste formula.
By the method, the corrosion behavior of the lead-acid storage battery made of different raw materials can be rapidly verified, the manufacturing method can be optimized at the initial stage of research and development, and data support is provided for scheme design.
Finally, it should be noted that: the above examples are only intended to illustrate the technical solution of the present invention, but not to limit it; although the present invention has been described in detail with reference to the foregoing embodiments, it will be understood by those of ordinary skill in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some technical features may be equivalently replaced; and such modifications or substitutions do not depart from the spirit and scope of the corresponding technical solutions of the embodiments of the present invention.
Claims (10)
1. A method for rapidly verifying the corrosion behavior of a lead-acid storage battery is characterized by comprising the following steps: the method comprises the following steps:
the method comprises the following steps: after positive and negative plates are respectively coated by diaphragms and combined into a plate group, the plate group to be tested is respectively placed in electrolytes with different concentrations for charging test, and the potential change condition and the charging quantity of the positive electrode in the charging process are recorded;
step two: soaking the charged positive plate in pure water, cleaning and drying, and detecting the thickness of the grid corrosion layer of the positive plate;
step three: and (4) placing the positive plate with the corrosion layer after the charging in the step one in electrolyte with the same concentration, and testing the conductivity of the corrosion layer at the interface of the positive plate.
2. The method for rapidly verifying the corrosion behavior of a lead-acid storage battery according to claim 1, characterized in that: in the first step, the alloy proportion of the positive plate is adjusted according to verification requirements.
3. The method for rapidly verifying the corrosion behavior of a lead-acid storage battery according to claim 1, characterized in that: the electrolyte selected in the step one is H2SO4And (3) an electrolyte.
4. The method for rapidly verifying the corrosion behavior of a lead-acid storage battery according to claim 1, characterized in that: and in the first step, the charging mode of the positive plate is a constant-voltage current-limiting charging mode.
5. The method for rapidly verifying the corrosion behavior of a lead-acid storage battery according to claim 1, characterized in that: the charging operation in the first step is as follows: positive and negative electrode plates, Hg/Hg2SO4The electrodes are respectively used as a working electrode, a counter electrode and a reference electrode to be connected with the electrochemical workstation, meanwhile, the positive plate and the negative plate are also respectively connected with the positive electrode and the negative electrode of the charging motor, and the measurement of the potential of the positive electrode and the measurement of the charging quantity in the charging process can be accurately known through a computer connected with the electrochemical workstation.
6. The method for rapidly verifying the corrosion behavior of a lead-acid storage battery according to claim 1, characterized in that: and in the second step, the positive plate is soaked in pure water, cleaned, dried, frozen and stored on the surface of the positive plate, and then the thickness of the grid corrosion layer is detected.
7. The method for rapidly verifying the corrosion behavior of a lead-acid battery according to claim 5, wherein the method comprises the following steps: and in the second step, the positive plate is soaked in pure water, washed, dried and then placed into liquid nitrogen for freezing to obtain a plate to be tested, and the thickness of the grid corrosion layer of the plate is tested by adopting SEM.
8. The method for rapidly verifying the corrosion behavior of a lead-acid storage battery according to claim 1, characterized in that: the specific operation of testing the conductivity of the corrosion layer on the interface of the positive plate in the third step is as follows: the positive plate is used as a working electrode, the large-area graphite plate is used as a counter electrode, and Hg/Hg is2SO4The positive plate and the large-area graphite plate are respectively connected with the positive electrode and the negative electrode of the charging motor, and the conduction condition of the corrosion layer on the interface of the positive plate is tested.
9. The method for rapidly verifying the corrosion behavior of a lead-acid storage battery according to claim 1, characterized in that: the electrolyte selected in the third step is H2SO4And (3) an electrolyte.
10. A system for rapidly verifying the corrosion behavior of a lead-acid battery, which is used for the method for rapidly verifying the corrosion behavior of the lead-acid battery in real time according to any one of claims 1 to 9, and comprises: the device comprises a positive plate (1), a negative plate (2), a battery jar (10), an electrochemical workstation (11) and a charging motor (21);
the positive plate (1) and the negative plate (2) are respectively coated by a diaphragm (3) and combined into a plate group; the pole group is arranged in the electrolyte (4) of the battery jar (10);
a positive plate (1), a negative plate (2) and Hg/Hg2SO4The electrodes are respectively used as a working electrode, a counter electrode and a reference electrode to be connected with an electrochemical workstation (11), and meanwhile, the positive plate (1) and the negative plate (2) are respectively connected with a positive electrode (8) and a negative electrode (9) of a charging motor (21).
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202010324044.5A CN111505520A (en) | 2020-04-22 | 2020-04-22 | Method and system for rapidly verifying corrosion behavior of lead-acid storage battery |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN202010324044.5A CN111505520A (en) | 2020-04-22 | 2020-04-22 | Method and system for rapidly verifying corrosion behavior of lead-acid storage battery |
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