CN115377429A - Surface treatment process for tubular grid of lead-acid battery - Google Patents

Surface treatment process for tubular grid of lead-acid battery Download PDF

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Publication number
CN115377429A
CN115377429A CN202210698790.XA CN202210698790A CN115377429A CN 115377429 A CN115377429 A CN 115377429A CN 202210698790 A CN202210698790 A CN 202210698790A CN 115377429 A CN115377429 A CN 115377429A
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lead
surface treatment
tubular grid
grid
acid battery
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Inventor
陈龙霞
唐胜群
李艳芬
战祥连
吴涛
武怀强
李敏
王玉莹
杨涛
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Zibo Torch Energy Co ltd
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    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00—Electrodes
    • H01M4/02—Electrodes composed of, or comprising, active material
    • H01M4/64—Carriers or collectors
    • H01M4/70—Carriers or collectors characterised by shape or form
    • H01M4/72—Grids
    • H01M4/73—Grids for lead-acid accumulators, e.g. frame plates
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00—Electrodes
    • H01M4/02—Electrodes composed of, or comprising, active material
    • H01M4/64—Carriers or collectors
    • H01M4/66—Selection of materials
    • H01M4/661—Metal or alloys, e.g. alloy coatings
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00—Electrodes
    • H01M4/02—Electrodes composed of, or comprising, active material
    • H01M4/64—Carriers or collectors
    • H01M4/66—Selection of materials
    • H01M4/665—Composites
    • H01M4/667—Composites in the form of layers, e.g. coatings
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00—Electrodes
    • H01M4/02—Electrodes composed of, or comprising, active material
    • H01M4/64—Carriers or collectors
    • H01M4/66—Selection of materials
    • H01M4/68—Selection of materials for use in lead-acid accumulators
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00—Electrodes
    • H01M4/02—Electrodes composed of, or comprising, active material
    • H01M4/64—Carriers or collectors
    • H01M4/82—Multi-step processes for manufacturing carriers for lead-acid accumulators
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
    • Y02E60/10—Energy storage using batteries

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Electrochemistry (AREA)
  • General Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Composite Materials (AREA)
  • Cell Electrode Carriers And Collectors (AREA)

Abstract

The invention relates to the technical field of grid surface treatment, in particular to a surface treatment process for a tubular grid of a lead-acid battery. The surface treatment process of the tubular grid of the lead-acid battery comprises the steps of soaking the tubular grid in a pre-prepared porous membrane mixed solution, and then preserving heat for 0.5-1 h in a nitrogen environment at 300-340 ℃ to obtain the tubular grid with the surface connected with a porous loose metal lead structure, namely finishing the surface treatment of the tubular grid; the pre-pore membrane mixed solution comprises the following raw materials in percentage by weight: 6-18% of micron-sized lead powder, 6-18% of magnesium dihydride, 6-26% of isopropylamine, 0.5-2% of carbomer resin and 60-65% of absolute ethyl alcohol. The surface treatment process for the tubular grid of the lead-acid battery solves the problem that the surface of a pressure casting tubular grid for the lead-acid battery is smooth and difficult to solidify, and simultaneously remarkably improves the quick charging performance of a paste squeezing tubular battery.

Description

Surface treatment process for tubular grid of lead-acid battery
Technical Field
The invention relates to the technical field of grid surface treatment, in particular to a surface treatment process for a tubular grid of a lead-acid battery.
Background
The tubular positive electrode structure adopted by the lead-acid storage battery effectively inhibits the failure of the battery caused by softening and falling of the positive electrode active substance, and the manufacturing method of the tubular positive electrode of the lead-acid storage battery is changed from the traditional dry powder filling type to the wet paste extruding type or the grouting type along with the requirement of environmental protection.
The tubular positive grid generally adopts a casting process of pressure casting, and compared with a grid cast by gravity, the surface of the rib is smoother. According to the traditional dry powder filling anode, a large number of large-aperture structures can be formed inside active substances in the subsequent pickling process, so that oxygen can enter the active substances during curing, the combination of a grid and the active substances is strengthened, the diffusion of electrolyte is facilitated in the use process of the battery, and the performance of the battery is improved. After wet paste squeezing or grouting is adopted, the porosity and the pore diameter inside the active substance are obviously reduced, the curing difficulty is high, the diffusion resistance of sulfuric acid inside the active substance is suddenly increased, and the performance is obviously reduced.
Disclosure of Invention
The technical problem to be solved by the invention is as follows: the surface treatment process for the tubular grid of the lead-acid battery solves the problem that the surface of a pressure casting tubular grid for the lead-acid battery is smooth and difficult to solidify, and simultaneously, the quick charging performance of the paste extrusion tubular battery is obviously improved.
The surface treatment process of the tubular grid of the lead-acid battery comprises the steps of soaking the tubular grid in a pre-perforated film mixed solution, and then preserving heat for 0.5-1 h in a nitrogen environment at 300-340 ℃ to obtain the tubular grid with a porous loose metal lead structure connected to the surface, namely finishing the surface treatment of the tubular grid;
the pre-pore membrane mixed solution comprises the following raw materials in percentage by weight: 6-18% of micron-sized lead powder, 6-18% of magnesium dihydride, 6-26% of isopropylamine, 0.5-2% of carbomer resin and 60-65% of absolute ethyl alcohol.
In the invention, the preparation method of the pre-pore membrane mixed solution comprises the following steps:
dissolving magnesium dihydride in isopropylamine under nitrogen environment to obtain a solution A; dissolving carbomer resin in absolute ethyl alcohol to obtain a solution B; and mixing the solution A and the solution B, stirring at a high speed for dispersion, adding micron-sized lead powder, and stirring uniformly at a low speed to obtain the pre-formed porous membrane mixed solution.
Preferably, the high-speed stirring dispersion speed is 1800-2200 revolutions per minute, and the high-speed stirring dispersion time is 10-30min.
Preferably, the low-speed stirring speed is 400-500 r/min, and the low-speed stirring time is 20-30min.
Preferably, the pre-pore membrane mixed solution has a viscosity of 0.05 to 0.1 pas at 25 ℃. The pre-pore membrane mixed solution within the viscosity range can ensure that a thin liquid difference layer is soaked on the surface of the tubular positive grid, so that a porous structure with a certain thickness is formed.
Preferably, the lead content of the micron-sized lead powder is more than 99.9wt%, and the average grain diameter is between 5 and 15 microns.
Preferably, when the tubular grid is soaked in the pre-pore membrane mixed solution, the tubular grid is completely soaked in the pre-pore membrane mixed solution for 5 to 10 seconds and then is extracted.
In the pre-formed porous membrane mixed solution, the magnesium dihydride has the function of quickly releasing hydrogen in a high-temperature environment to form a porous structure; isopropylamine is used as a good solvent for magnesium dihydride and is used for dissolving the magnesium dihydride; absolute ethyl alcohol is used for dissolving the carbomer resin, so that the thickening effect of the mixed solution is achieved, and after micron lead powder is added, the uniform concentration of lead particles at each part of the solution is ensured.
In the invention, when the tubular grid is soaked in the pre-pore membrane mixed solution, the tubular grid is completely immersed in the pre-pore membrane mixed solution for 5-30s. The surface of the grid is dipped with a layer of pre-perforated membrane, and the smooth surface part of the grid is connected with a layer of porous loose metallic lead structure through high-temperature treatment.
In the invention, the preparation of the pre-pore-forming film and the impregnation of the grid are both carried out in a nitrogen environment, so that the problem that magnesium dihydride is decomposed too early to influence the pore-forming effect at high temperature in the later period is avoided. The temperature of the high-temperature device is set to be within the range of 300-340 ℃, and the high-temperature device is kept for 0.5-1 h, so that the anhydrous ethanol, the isopropylamine and the carbomer resin are guaranteed to be decomposed, and meanwhile, the micron-sized lead powder is fused with the grid substrate, and the porous structure is not damaged.
Compared with the prior art, the invention has the following beneficial effects:
the invention combines the curing mechanism and the characteristics of porous lead, and connects a layer of porous loose metallic lead structure on the surface of a smooth pressure casting grid, thereby reducing the difficulty of combining the grid and active substances in the curing process, improving the conductivity of the grid and the active substances, solving the problem that the surface of a pressure casting tubular grid for a lead-acid battery is smooth and difficult to cure, and simultaneously obviously improving the quick charging performance of a paste extrusion tubular battery.
Drawings
FIG. 1 is a schematic view of the structure of tubular grid ribs after surface treatment according to the present invention;
fig. 2 is a comparison of the combination of the tubular grid ribs and the lead paste after the surface treatment and the combination of the tubular grid ribs and the lead paste without the surface treatment in example 1; wherein, a is after surface treatment, b is without surface treatment;
fig. 3 is a comparison of terminal voltage during formation of a tubular grid simulated battery after surface treatment and terminal voltage during formation of a tubular grid simulated battery without surface treatment in example 1 of the present invention; wherein, a is after surface treatment, b is without surface treatment;
FIG. 4 is a schematic cross-sectional view of a tubular grid after formation in accordance with example 1 of the present invention;
in the figure: 1. grid ribs; 2. a porous lead structure layer; 3. and corroding the layer.
Detailed Description
The present invention will be further described with reference to the following examples, which are not intended to limit the practice of the present invention.
Example 1
Preparing a pre-pore membrane mixed solution:
in a glove box, 50g of magnesium dihydride powder was weighed into beaker A, and 200g of isopropylamine solution was added and stirred well until the powder was completely dissolved to give solution A. And adding 5g of carbomer resin into the beaker B, adding 490g of absolute ethyl alcohol, and stirring until the carbomer resin is completely dissolved to obtain a solution B. And mixing the solution A and the solution B, shearing and stirring by using high-speed dispersion equipment at the rotating speed of 1800 rpm for 30min, and adding 50g of pure lead powder with the average particle size of 10 microns, wherein the purity is 99.9%. The rotation speed is adjusted to 400 r/min, stirring is continued for 20min until the transparency of each part of the solution is consistent, and the viscosity of the mixed solution is measured by using a viscometer and is 0.08 Pa.s.
Carrying out surface treatment on the tubular grid:
and completely immersing the pressure cast tubular traction lead-acid storage battery D50 positive grid into the pre-pore membrane mixed solution in a glove box for 5s, then taking out, quickly putting into a high-temperature device filled with nitrogen at 300 ℃, and preserving heat for 0.5h to obtain a tubular grid with a porous loose metal lead structure connected to the surface, namely finishing the surface treatment of the tubular grid.
And (3) comparing the performance index test of the tubular grid after surface treatment with that of the tubular grid without surface treatment, wherein the performance index test specifically comprises the following steps:
(1) Combining the grid and the terylene calandria with apparent density of 3.8g/cm 3 The positive lead plaster is extruded into a cavity between a grid rib and a calandria, and enters a curing device for curing to obtain a polar plate, and the curing and drying methods are shown in table 1:
TABLE 1 curing, drying Process parameters
Figure BDA0003703154200000031
After curing, the plate is dissected, the bonding condition of the grid ribs and the lead paste is observed and processed, and is compared with the bonding condition of the grid ribs and the lead paste which are not subjected to surface treatment, and the figure 2 shows. As can be seen from fig. 2, after the grid is subjected to surface treatment by the treatment method of the present invention, good connection is established between the ribs and the lead paste during curing, and more lead paste is attached to the surfaces of the ribs, so that the curing difficulty is reduced.
(2) The method for assembling the grid plate simulation battery with the surface treated by the invention comprises the following steps:
two groups of simulation batteries are assembled by 1D 50 type positive green plate assembled by using the grid after surface treatment and 2D 50 type negative green plates of the lead-acid storage battery for traction, a PE polyethylene clapboard is used for coating the negative plate, the distances between the positive green plate and the negative green plates at two sides are both 1cm, and 1.06g/ml sulfuric acid electrolyte is filled for formation.
Meanwhile, a reference simulation battery is prepared by the following method:
two groups of simulation batteries are assembled by 1D 50 type positive green plate manufactured by a traditional paste squeezing mode and 2D 50 type negative green plates of the lead-acid storage battery for traction, a PE polyethylene clapboard is used for coating the negative plate, the distance between the positive green plate and the negative green plates at two sides is 1cm, and 1.06g/ml sulfuric acid electrolyte is filled for formation.
The two types of simulated batteries are formed by the following method:
the first step is as follows: 3A,1h;
the second step: 10A,4h;
the third step: 6A,15h.
The terminal voltages during formation of the two simulated cells after formation are shown in fig. 3. As can be seen from fig. 3, the voltage of the simulated battery terminal of the grid treated by the surface treatment process of the present invention is significantly lower than that of the reference electrode during formation, which indicates that the electronic connection between the ribs and the lead paste is good, and the polarization of the electrode during formation is reduced.
(3) The cross section of the grid rib treated by the surface treatment process is observed, and the figure is shown in figure 4. As can be seen in fig. 4, the surface of the ribs has a rough surface with an erosion layer attached to the outside of the rough surface that is formed during the formation.
(4) The electrolyte of a group of the simulation battery and the reference simulation battery is quickly changed into 1.28g/ml sulfuric acid electrolyte, and after the supplementary charging is carried out for 4 hours by using the current of 3.5A, the discharging test is carried out.
And (3) capacity testing:
discharging at 10A, stopping the voltage at 1.70V, and normally charging;
50A (1C) is discharged, the voltage is stopped to be 1.50V, and the charging is normal.
The normal charging method comprises the following steps: 7A charging, limiting the voltage to 2.4V, and then turning to 3.5A charging for 12h.
And (3) testing the charging acceptance capacity:
the charged battery was discharged again at 10A, and after the voltage was terminated at 1.70V, the battery was charged at a large current of 50A, and the time from the terminal voltage of the battery to 2.45V was recorded to examine the charge acceptance of the battery.
And (3) resistance testing:
fully charged simulated battery resistance was tested using an american Arbin device with parameters set:
pulse current 10A, time 5ms.
The test results are shown in Table 2.
Table 2 simulated battery test results
Name (R) The invention simulates a battery Reference analog battery
10A discharge time/h 6.5 6.6
50A (1C) discharge time/min 55 49
50A charging time reaching 2.45V/h 45 33
Resistance/m omega 1.5 3.9
As can be seen from Table 2, the discharge capacity of the simulated battery 10A is equivalent to that of the reference, but the discharge performance, the charge acceptance and the resistance of the large-current 1C simulated battery are all superior to those of the reference simulated battery.
Example 2
Preparing a pre-pore membrane mixed solution:
in a glove box, 100g of magnesium dihydride powder was weighed into a beaker A, and 50g of isopropylamine solution was added and stirred well until the powder was completely dissolved to obtain a solution A. After 10g of carbomer resin was placed in beaker B, 400g of absolute ethanol was added and stirred until the resin was completely dissolved to obtain solution B. Mixing the solution A and the solution B, shearing and stirring by using high-speed dispersion equipment at the rotating speed of 2200 revolutions per minute, and adding 100g of pure lead powder with the average grain diameter of 15 microns after 10 minutes, wherein the purity is 99.9 percent. The rotation speed is adjusted to 500 revolutions per minute, stirring is continued for 30 minutes until the transparency of each part of the solution is consistent, and the viscosity of the mixed solution is measured by a viscometer, wherein the viscosity value is 0.075 Pa.s.
Carrying out surface treatment on the tubular grid:
and (3) completely immersing the pressure cast tubular traction lead-acid storage battery D50 positive grid into the pre-perforated membrane mixed solution in a glove box for 10s, then taking out, quickly putting into a high-temperature device filled with nitrogen and at 340 ℃, preserving heat for 1h, obtaining a tubular grid with a porous loose metal lead structure connected to the surface, namely finishing surface treatment of the tubular grid, and preparing 27 grids.
And (3) comparing the performance index test of the tubular grid after surface treatment with that of the tubular grid without surface treatment, wherein the method specifically comprises the following steps:
combining the grid and the terylene calandria after surface treatment, and observing the densityDegree of 3.82g/cm 3 The positive lead plaster is extruded into a cavity between the grid ribs and the calandria, and enters a curing device for curing to obtain the polar plate, and the curing and drying methods are shown in table 1.
Three D-450 lead-acid storage batteries for traction are assembled by adopting a 9 plus 10 minus pole group structure and a PE separator coated negative pole design for 1 paste-extruded tubular positive green plate prepared by using the grid subjected to surface treatment, and the design is compared with the traditional paste-extruded D-450 lead-acid battery after formation.
The two batteries are formed in the same batch by using an acid circulation forming method, wherein the acid circulation method comprises the following steps:
firstly, an acid circulation low-density system is opened, and the density of low-density electrolyte is adjusted to 1.060g/cm 3 -1.080g/cm 3 In the range, the battery injection port is connected with the connector for acid circulation, at the moment, low-density electrolyte flows into the single battery through the connector to start acid injection, the single battery is soaked for 2 hours in a circulating mode after the acid injection is finished, then the acid circulation system is started to be connected with a power supply to start charging, and a control program of a computer formation device is started to perform charging formation. In the low-density circulation process, the density of low-density electrolyte in the high-order acid tank flows into an acid circulation system through a certain pressure, the acid circulation system flows into an acid inlet pipe of an acid circulation connector through an acid inlet pipeline so as to enter the interior of the battery, and then returns to an acid return pipeline from an acid return pipe of the acid circulation connector and flows into a low-order tank.
And before the acid circulation formation program is operated to the beginning of the last stage, closing the low-density acid liquid circulation system, opening the high-density acid liquid circulation system, and starting circulation acid change. And adjusting according to the measurement result until the acid liquid density reaches (1.290 +/-0.005) g/cm 3 (30 ℃) and is stable for 0.5 h. And (5) ending the acid circulation formation charging stage, closing the cooling system and taking down the acid circulation connector.
Performance tests were performed on two batteries:
(1) 5hr capacity test, discharge current 90A, end voltage 1.7V, record discharge time;
(2) Performing high-rate discharge test, discharging at 450A, stopping at 1.5V, and recording discharge time;
(3) The high current charge test, 450A (1C), was performed with charging, the time to 2.45V recorded, and the electrolyte temperature in the cell recorded.
(4) Resistance test, the battery that finishes to charging carries out resistance test, and the parameter sets for:
pulse current 30A, time 5ms.
The test results are shown in Table 3.
TABLE 3
Item Reference cell Battery of the present application
5hr discharge time/h 4.98h 5.19h
450A discharge time/min 37 46
1C charging to 2.45V time/min 36 42
Highest temperature/deg.C on 1C charge 38.5 33
Resistance/m omega 11.5 7.6
As can be seen from table 3, the cells of the present invention have superior high current 1C discharge performance, charge acceptance, and resistance to the reference simulated cell.

Claims (9)

1. A surface treatment process for a tubular grid of a lead-acid battery is characterized by comprising the following steps: soaking the tubular grid in the pre-pore membrane mixed solution, and then preserving heat for 0.5h-1h in a nitrogen environment at 300-340 ℃ to obtain the tubular grid with the surface connected with a porous loose metallic lead structure, namely finishing surface treatment on the tubular grid;
the pre-pore membrane mixed solution comprises the following raw materials in percentage by weight: 6-18% of micron-sized lead powder, 6-18% of magnesium dihydride, 6-26% of isopropylamine, 0.5-2% of carbomer resin and 60-65% of absolute ethyl alcohol.
2. The surface treatment process for the tubular grid of the lead-acid battery according to claim 1, characterized by comprising the following steps of: the preparation method of the pre-pore membrane mixed solution comprises the following steps:
dissolving magnesium dihydride in isopropylamine under nitrogen environment to obtain a solution A; dissolving carbomer resin in absolute ethyl alcohol to obtain a solution B; and mixing the solution A and the solution B, stirring at a high speed for dispersion, adding micron-sized lead powder, and stirring uniformly at a low speed to obtain the pre-formed porous membrane mixed solution.
3. The surface treatment process of the tubular grid of the lead-acid battery according to claim 2, characterized in that: the high-speed stirring dispersion speed is 1800-2200 r/min.
4. The surface treatment process for the tubular grid of the lead-acid battery according to claim 2, characterized in that: the high-speed stirring dispersion time is 10-30min.
5. The surface treatment process of the tubular grid of the lead-acid battery according to claim 2, characterized in that: the low-speed stirring speed is 400-500 r/min.
6. The surface treatment process of the tubular grid of the lead-acid battery according to claim 2, characterized in that: the low-speed stirring time is 20-30min.
7. The surface treatment process for the tubular grid of the lead-acid battery according to claim 1 or 2, characterized in that: the viscosity of the pre-pore membrane mixed solution at 25 ℃ is 0.05-0.1 Pa.s.
8. The surface treatment process of the tubular grid of the lead-acid battery according to claim 1 or 2, characterized in that: the lead content of the micron-sized lead powder is more than 99.9wt%, and the average grain diameter is between 5 and 15 micrometers.
9. The surface treatment process for the tubular grid of the lead-acid battery according to claim 1, characterized by comprising the following steps of: and when the tubular grid is soaked in the pre-pore membrane mixed solution, completely soaking the tubular grid in the pre-pore membrane mixed solution for 5-10s, and then extracting.
CN202210698790.XA 2022-06-20 2022-06-20 Surface treatment process for tubular grid of lead-acid battery Pending CN115377429A (en)

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