CN111595761A - Method for testing corrosion resistance of positive plate grid - Google Patents
Method for testing corrosion resistance of positive plate grid Download PDFInfo
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- CN111595761A CN111595761A CN201910287592.2A CN201910287592A CN111595761A CN 111595761 A CN111595761 A CN 111595761A CN 201910287592 A CN201910287592 A CN 201910287592A CN 111595761 A CN111595761 A CN 111595761A
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- 230000007797 corrosion Effects 0.000 title claims abstract description 98
- 238000005260 corrosion Methods 0.000 title claims abstract description 98
- 238000012360 testing method Methods 0.000 title claims abstract description 46
- 238000000034 method Methods 0.000 title claims abstract description 20
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 30
- 238000003466 welding Methods 0.000 claims abstract description 20
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims abstract description 14
- 239000007788 liquid Substances 0.000 claims abstract description 14
- 238000005303 weighing Methods 0.000 claims abstract description 13
- 238000003860 storage Methods 0.000 claims abstract description 12
- 230000004580 weight loss Effects 0.000 claims abstract description 10
- 238000001035 drying Methods 0.000 claims abstract description 9
- 239000003513 alkali Substances 0.000 claims abstract description 7
- 238000007789 sealing Methods 0.000 claims abstract description 4
- 239000000523 sample Substances 0.000 claims description 13
- 239000003792 electrolyte Substances 0.000 claims description 11
- 238000005520 cutting process Methods 0.000 claims description 9
- 238000010998 test method Methods 0.000 claims description 9
- 239000012496 blank sample Substances 0.000 claims description 8
- 238000002791 soaking Methods 0.000 claims description 7
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 6
- 239000008399 tap water Substances 0.000 claims description 6
- 235000020679 tap water Nutrition 0.000 claims description 6
- 238000005406 washing Methods 0.000 claims description 6
- 239000002253 acid Substances 0.000 claims description 5
- 239000008367 deionised water Substances 0.000 claims description 5
- 229910021641 deionized water Inorganic materials 0.000 claims description 5
- 238000005192 partition Methods 0.000 claims description 5
- 238000001514 detection method Methods 0.000 claims description 3
- 239000002932 luster Substances 0.000 claims description 3
- CZMRCDWAGMRECN-UGDNZRGBSA-N Sucrose Chemical compound O[C@H]1[C@H](O)[C@@H](CO)O[C@@]1(CO)O[C@@H]1[C@H](O)[C@@H](O)[C@H](O)[C@@H](CO)O1 CZMRCDWAGMRECN-UGDNZRGBSA-N 0.000 claims description 2
- 229930006000 Sucrose Natural products 0.000 claims description 2
- 239000002585 base Substances 0.000 claims description 2
- 238000001291 vacuum drying Methods 0.000 claims description 2
- 238000011156 evaluation Methods 0.000 claims 1
- 239000011259 mixed solution Substances 0.000 claims 1
- 239000000243 solution Substances 0.000 claims 1
- 229960004793 sucrose Drugs 0.000 claims 1
- 238000012544 monitoring process Methods 0.000 abstract description 3
- 238000005266 casting Methods 0.000 abstract 1
- 238000005868 electrolysis reaction Methods 0.000 description 4
- 230000002159 abnormal effect Effects 0.000 description 3
- 230000007547 defect Effects 0.000 description 3
- 230000007613 environmental effect Effects 0.000 description 2
- 229910000978 Pb alloy Inorganic materials 0.000 description 1
- 239000013543 active substance Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 239000001999 grid alloy Substances 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 230000000717 retained effect Effects 0.000 description 1
- 239000005720 sucrose Substances 0.000 description 1
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N17/00—Investigating resistance of materials to the weather, to corrosion, or to light
- G01N17/006—Investigating resistance of materials to the weather, to corrosion, or to light of metals
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N5/00—Analysing materials by weighing, e.g. weighing small particles separated from a gas or liquid
- G01N5/04—Analysing materials by weighing, e.g. weighing small particles separated from a gas or liquid by removing a component, e.g. by evaporation, and weighing the remainder
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Abstract
A method for testing corrosion resistance of positive plate grid includes weighing cut positive plate grid and negative plate grid, recording weight data of each positive plate grid, and marking serial number; and the positive grids and the negative grids sleeved with the separators are alternately stacked and tidily arranged to form a grid cluster. Casting and welding the grid cluster and loading the grid cluster into a storage battery tank; carrying out butt welding and heat sealing on the grid clusters; and preparing the corrosion-resistant sample piece of the plate grid. And injecting a sulfuric acid solution into each cell of the grid corrosion-resistant sample piece, connecting the grid corrosion-resistant sample piece to a test loop, and performing corrosion test in a constant-current mode or a constant-voltage mode. And after the corrosion test is finished, taking out the positive grid, putting the positive grid into the sugar-alkali water corrosive liquid to remove the corrosion layer on the surface of the positive grid, drying, and weighing and recording piece by piece. And (4) calculating the weight loss proportion or unit area corrosion rate of the positive grid after corrosion, and evaluating the corrosion resistance of the positive grid. The invention can effectively prevent the distortion of the test result caused by the short circuit of the grid by monitoring the abnormity in the corrosion test process.
Description
Technical Field
The invention belongs to the technical field of lead-acid storage batteries, and particularly relates to a method for testing corrosion resistance of a positive grid.
Background
The grid is a support carrier for the active substance of the lead-acid storage battery and also plays a role in conducting current in the charging and discharging processes. The positive plate grid can be gradually corroded in the using process of the storage battery, and the service life and the low-temperature discharge performance of the storage battery are seriously influenced after the positive plate grid is corroded or the ribs of the plate grid are corroded and broken.
The current universal method for testing and evaluating the corrosion resistance of the positive grid mainly comprises a high-temperature service life test, such as a SAEJ2801 test, a SAE J240 test, a 60 ℃ water loss test and the like. However, the test method has two defects in evaluating the corrosion resistance of the positive grid: firstly, the testing period is long, and generally 4 to 6 months are needed; secondly, the corrosion resistance of the positive plate grid is only a factor influencing the high-temperature service life, particularly for a lean solution AGM battery, the service life times are the performance of the combined action of multiple influencing factors, and the corrosion resistance of the positive plate grid cannot be directly evaluated according to the service life times.
Patent CN 104075960B discloses a method for rapidly measuring corrosion resistance of a storage battery grid alloy, which mainly comprises the following steps: weighing a grid with the corrosion resistance to be measured; the grid is used as the anode, other materials with the same area and any conductivity and corrosion resistance are used as the cathode to form an electrolysis loop, and the electrolysis loop is connected with a lead and put into an electrolysis bath; adding a sulfuric acid solution into an electrolytic cell, and placing the electrolytic cell in a constant-temperature water bath box; connecting an electrolysis loop to a charge and discharge machine, and performing constant current corrosion and charge and discharge circulation; taking down the positive grid, soaking in boiling sugar alkali solution, and stripping off corrosion products; and drying and weighing the positive grid stripped by the corrosion product, calculating a weight difference value before and after the grid is corroded, and calculating the weight loss rate of the grid according to the weight difference value. The method has the following defects: the positive plate grid and the negative plate grid are not effectively blocked, so that the contact short circuit of the positive and negative electrodes cannot be prevented, different positive plate grids respectively form an electrolytic loop, and the test error caused by the difference between the loops cannot be avoided; adding a sulfuric acid solution into the electrolytic bath to enable the liquid level of the sulfuric acid solution to be slightly higher than the top end of the grid, but the liquid level can be reduced in the test process, so that part of the grid can be exposed out of the liquid level; the boiled sugar alkaline water can dissolve corrosion products and corrode the lead alloy matrix of the grid, and the method does not consider the influence of the factors and the like.
Disclosure of Invention
In order to overcome the defects in the background art, the invention aims to provide a scientific and effective positive grid corrosion resistance performance testing method which can accurately calculate the corrosion resistance performance of a positive grid and effectively prevent the distortion of a testing result caused by grid short circuit.
The technical scheme of the invention comprises the following steps:
the method is characterized by comprising the following steps:
1) taking a cut positive grid and a cut negative grid, wherein the sizes of the positive grid and the negative grid are matched; weighing and recording weight data m of each positive grid1And the plate lug positions are marked with serial numbers; taking 4-10 positive grids in the same batch, cutting off the lug edges of the positive grids at the position flush with the upper frame of the grids, and recording the average weight m of the cut lugs21-3 pieces of positive grids with cut lugs are reserved for standby;
2) alternately stacking the positive grids and the negative grids to form a grid cluster;
3) welding homopolar grids in the single grid cluster through the busbars, and connecting the homopolar grids in the single grid cluster in parallel; then, placing the grid clusters into a storage battery cell according to the sequence that the anode bus bar and the cathode bus bar of the adjacent clusters are connected, wherein one group of grid clusters corresponds to one storage battery cell;
4) carrying out butt welding on busbars between adjacent single grids of the grid clusters filled in the battery tank body, wherein the grid clusters of all the single grids are connected in series; detecting the butt welding quality and whether the grid cluster is short-circuited, and thermally sealing the battery cover and the welding terminal after the detection is qualified to prepare a grid corrosion-resistant sample piece;
5) injecting a sulfuric acid solution with the concentration of 1.300 +/-0.020 g/ml (25 ℃) into each unit cell of the grid corrosion-resistant sample piece until the bus bar is just submerged, and adding acid in each unit cell +/-5 ml; then connecting the grid corrosion-resistant sample piece with a test loop, and carrying out corrosion test according to a constant current mode or a constant voltage mode:
a constant current mode: corroding for T hours in a constant-temperature water bath at 40-75 ℃ by using a constant current of 2-4A;
constant pressure mode: performing constant-pressure corrosion for T hours in a constant-temperature water bath tank at the temperature of 60-75 ℃ and at the constant pressure of 15.6 +/-1.0V;
6) after the corrosion test is finished, dissecting a battery cover, cutting off butt welding points connected with each unit grid, taking out a grid cluster in each unit grid, disassembling a partition plate sleeved on the grid, washing residual electrolyte on the surface of the grid for 5-15 minutes by using tap water, and then soaking in pure water for 2-5 hours;
7) cutting the positive grid from the welding position of the lug and the busbar, then putting the positive grid into a sugar-alkali water corrosive liquid, and removing the corrosion layer on the surface of the positive grid until the surface of the positive grid is completely exposed with metallic luster; when the corrosion layer is removed, 1-3 positive grids of the cut plate lugs reserved in the same batch are placed as blank samples for comparison, and the weight m of each blank positive grid before being placed in the corrosion liquid is recordedk1(ii) a Washing the positive grid with tap water to remove the surface corrosion layer, wherein the surface of the positive grid comprises a blank sample for 5-15 minutes, and then soaking in pure water for 1-3 hours;
8) drying the positive plate grid for 30-60 minutes by using a drying oven at the set temperature of 60 +/-10 ℃, and weighing and recording the weight m of each positive plate grid3And correspondingly marking according to serial number marks made at the plate lug positions, weighing and recording the dry weight m of each blank positive plate grid after the corrosion layer is removedk2(ii) a Calculating blank comparison parameter £= (m)k2- mk1)* m3/(m1-m2)；
9) Calculating weight loss ratio of positive grid after corrosion = [ (m)1-m2)-m3+￡]/(m1-m2) 100% of the total weight; positive grid unit area corrosion rate = = [ (m)1-m2)-m3+￡]And S/T, evaluating the corrosion resistance of the positive plate grid according to the calculated data, wherein S is the surface area of the positive plate grid without the plate lug.
In the step 2), 3-6 positive grids are preferably selected in each grid cluster, more negative grids are selected than the positive grids, and the outermost grids on two sides of the grid cluster are negative grids.
In the step 2), the negative grid is sleeved with a PE separator or an AGM separator, or the positive grid and the negative grid are sleeved with the PE separator or the AGM separator.
In the step 5) of the invention, a constant current of 2-4A is used for corrosion for T hours in a constant temperature water bath of 40-75 ℃, wherein T is 300-.
The step 5) of the invention is to carry out constant pressure corrosion for T hours in a constant temperature water bath tank at the temperature of 60-75 ℃ and at the constant pressure of 15.6 +/-1.0V, wherein T is 300-.
In the step 5) of the invention, the electrolyte level of the cell is regularly observed in the corrosion test process, deionized water is timely supplemented into the cell, and the electrolyte level is maintained to be flush with the busbar; and regularly observing the overflow condition of bubbles in the cells, and stopping the test when no bubble emerges from a certain cell; or the charging voltage and the charging current curve of the grid corrosion-resistant sample piece are checked and compared regularly, when the charging voltage in a constant current mode drops suddenly or the charging current in a constant voltage mode rises suddenly, the test is stopped, and the regular mode is as follows: 20 hours, 24 hours, 30 hours.
The weight ratio of the sugar-containing aqueous alkali corrosive liquid in the step 7) of the invention to the sucrose, the sodium hydroxide and the deionized water is (1-3): (3-5): (30-50), wherein the dosage of the sugar-base aqueous corrosion solution is 3-8 times of the weight of the grid.
In the step 8), the positive plate grid is dried by using a vacuum drying oven.
Furthermore, the corrosion test time T hour in the fifth step is empirical data, the selected constant current value or constant voltage value is higher, and the T is correspondingly reduced; the temperature of the selected water bath is higher or the number of the grids of each grid cluster is less, and T is correspondingly reduced.
Furthermore, the weight loss proportion of the positive grid in the step ninthly is controlled to be between 15 and 35 percent, and the corrosion test conditions such as the corrosion test time, the selected constant current value or constant voltage value, the constant temperature water bath temperature and the like in the step fifthly can be controlled.
The invention has the beneficial effects that: according to the invention, the positive grids needing to be subjected to corrosion resistance comparison can be brought into the same grid corrosion resistance sample piece, even the same grid cluster and the same battery cell unit grid, so that the grids with the same polarity in a single grid cluster are connected in parallel, and the grid clusters of all the unit grids are connected in series, thereby effectively avoiding the deviation caused by the individual difference of test samples, the difference of external circuits, the difference of connection resistance of wires, the temperature or concentration of electrolyte in which the grids are positioned and other environmental differences; the invention can effectively prevent the distortion of the test result caused by the short circuit of the grid by monitoring the abnormity in the corrosion test process; the blank sample contrast parameters introduced by the invention are convenient for calculating the corrosion resistance of the positive grid more accurately.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below in conjunction with the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, rather than all embodiments, and all other embodiments obtained by a person of ordinary skill in the art without creative efforts based on the embodiments of the present invention belong to the protection scope of the present invention.
Examples
The same structure of A, B, C, D, E five types of positive grids requires comparison of corrosion resistance, and the detailed test method is as follows:
and secondly, sheathing the PE partition plates on the positive plate grids, and forming plate grid clusters after the positive plate grids and the negative plate grids sheathed with the partition plates are alternately and orderly stacked, wherein 6 plate grid clusters are formed. Each grid cluster comprises 5 positive grids and 6 negative grids, and 5 positive grids in a single grid cluster correspond to 5 types;
observing the electrolyte level of the unit grids every 24 hours, replenishing deionized water into the unit grid electric tank in time, and maintaining the electrolyte level to be flush with the busbar; observing the overflow condition of bubbles in the cells, and when no bubble emerges from a certain cell, terminating the test and recording the actual corrosion time;
Table 1 serial number of each positive grid and corresponding m1、m2、m3Data of
TABLE 2M corresponding to each type of blank positive gridk1、mk2Data of
TABLE 3 blank sample contrast parameter £ data for each type of positive plate grid
In general, calculation analysis is performed on the weight loss data of all positive grids, and if obvious abnormal data exist, the abnormal data are removed for analysis and comparison again. After the abnormal 1 st cell and 6 th cell are removed from the group of data, the average value of the weight loss ratio is as follows:
table 4 weight loss ratio of each type of positive grid
Namely A, B, C, D, E five types of positive grids with the same structure, the weight loss ratio D is more than B and more than C and more than A and less than E, the corrosion resistance D of the positive grid is optimal, and the E is worst.
According to the invention, the positive grids needing to be subjected to corrosion resistance comparison are brought into the same grid corrosion resistance sample piece, even the same grid cluster and the same battery cell unit grid, so that the grids with the same polarity in a single grid cluster are connected in parallel, and the grid clusters of all the unit grids are connected in series, thereby effectively avoiding test deviation caused by environmental differences such as individual difference of test samples, difference of external circuits, temperature or concentration of electrolyte in the grids and the like; the invention can effectively prevent the distortion of the test result caused by the short circuit of the grid by monitoring the abnormity in the corrosion test process; the blank sample contrast parameters introduced by the invention are convenient for calculating the corrosion resistance of the positive grid more accurately.
The method for testing the corrosion resistance of the positive grid provided by the embodiment of the invention is described in detail, a specific example is applied to explain the principle and the implementation mode of the invention, and the description of the embodiment is only used for helping to understand the method and the core idea of the invention; meanwhile, for a person skilled in the art, according to the idea of the present invention, there may be variations in the specific embodiments and the application scope, and in summary, the content of the present specification should not be construed as a limitation to the present invention.
Claims (8)
1. A method for testing corrosion resistance of a positive grid is characterized by comprising the following steps:
1) taking a cut positive grid and a cut negative grid, wherein the sizes of the positive grid and the negative grid are matched; weighing and recording weight data m of each positive grid1And the plate lug positions are marked with serial numbers; taking another positive grid 4-10 of the same batch, cutting off the lug edge of the positive grid at the position flush with the upper frame of the grid, and recording the average weight m of the cut lug21-3 pieces of positive grids with cut lugs are reserved for standby;
2) alternately stacking the positive grids and the negative grids to form a grid cluster;
3) welding homopolar grids in the single grid cluster through the busbars, and connecting the homopolar grids in the single grid cluster in parallel; then, placing the grid clusters into a storage battery cell according to the sequence that the anode bus bar and the cathode bus bar of the adjacent clusters are connected, wherein one group of grid clusters corresponds to one storage battery cell;
4) carrying out butt welding on busbars between adjacent single grids of the grid clusters filled in the battery tank body, wherein the grid clusters of all the single grids are connected in series; detecting the butt welding quality and whether the grid cluster is short-circuited, and thermally sealing the battery cover and the welding terminal after the detection is qualified to prepare a grid corrosion-resistant sample piece;
5) injecting a sulfuric acid solution with the concentration of 1.300 +/-0.020 g/ml (25 ℃) into each unit cell of the grid corrosion-resistant sample piece until the bus bar is just submerged, and adding acid in each unit cell +/-5 ml; then connecting the grid corrosion-resistant sample piece with a test loop, and carrying out corrosion test according to a constant current mode or a constant voltage mode:
a constant current mode: corroding for T hours in a constant-temperature water bath at 40-75 ℃ by using a constant current of 2-4A;
constant pressure mode: performing constant-pressure corrosion for T hours in a constant-temperature water bath tank at the temperature of 60-75 ℃ and at the constant pressure of 15.6 +/-1.0V;
6) after the corrosion test is finished, dissecting a battery cover, cutting off butt welding points connected with each unit grid, taking out a grid cluster in each unit grid, disassembling a partition plate sleeved on the grid, washing residual electrolyte on the surface of the grid for 5-15 minutes by using tap water, and then soaking in pure water for 2-5 hours;
7) cutting the positive grid from the welding position of the lug and the busbar, then putting the positive grid into a sugar-alkali water corrosive liquid, and removing the corrosion layer on the surface of the positive grid until the surface of the positive grid is completely exposed with metallic luster; when the corrosion layer is removed, 1-3 positive grids of the cut plate lugs reserved in the same batch are placed as blank samples for comparison, and the weight m of each blank positive grid before being placed in the corrosion liquid is recordedk1(ii) a Washing the positive grid with tap water to remove the surface corrosion layer, wherein the surface of the positive grid comprises a blank sample for 5-15 minutes, and then soaking in pure water for 1-3 hours;
8) drying the positive plate grids for 30-60 minutes by using a drying box at the set temperature of 60 +/-10 ℃, weighing and recording the weight m of each positive plate grid3And correspondingly marking according to serial number marks made at the plate lug positions, weighing and recording the dry weight m of each blank positive plate grid after the corrosion layer is removedk2(ii) a Calculating blank comparison parameter £= (m)k2- mk1)* m3/(m1-m2)；
9) Calculating weight loss ratio of positive grid after corrosion = [ (m)1-m2)-m3+￡]/(m1-m2) 100% of the total weight; positive grid unit area corrosion rate = = [ (m)1-m2)-m3+￡](S/T) evaluation of the data obtained from the calculationThe positive plate grid has corrosion resistance, and S is the surface area of the positive plate grid without plate lugs.
2. The positive grid corrosion resistance test method according to claim 1, characterized in that: in the step 2), 3-6 positive grids are preferably selected in each grid cluster, more negative grids are selected than the positive grids, and the outermost grids on two sides of the grid cluster are negative grids.
3. The positive grid corrosion resistance test method according to claim 1, characterized in that: and 2) sleeving a PE separator or an AGM separator on the negative grid in the step 2), or sleeving a PE separator or an AGM separator on both the positive grid and the negative grid.
4. The positive grid corrosion resistance test method according to claim 1, characterized in that: step 5) in a constant-temperature water bath tank at 40-75 ℃, using a constant current of 2-4A to corrode for T hours, wherein T is 300-600.
5. The positive grid corrosion resistance test method according to claim 1, characterized in that: step 5) carrying out constant-pressure corrosion for T hours in a constant-temperature water bath tank at the temperature of 60-75 ℃ at the constant pressure of 15.6 +/-1.0V, wherein T is 300-600-.
6. The positive grid corrosion resistance test method according to claim 1, characterized in that: step 5) periodically observing the liquid level of the electrolyte in the cells in the corrosion test process, replenishing deionized water to the cells in time, and maintaining the liquid level of the electrolyte to be flush with the busbar; and regularly observing the overflow condition of bubbles in the cells, and stopping the test when no bubble emerges from a certain cell; or regularly checking and comparing the charging voltage and charging current curves of the grid corrosion-resistant sample piece, and stopping the test when the charging voltage in a constant current mode is suddenly reduced or the charging current in a constant voltage mode is suddenly increased, wherein the regular time is as follows: 20 hours, 24 hours or 30 hours.
7. The positive grid corrosion resistance test method according to claim 1, characterized in that: the sugar-alkali water corrosive liquid in the step 7) is prepared from cane sugar, sodium hydroxide and deionized water in a weight ratio of 1-3: 3-5: 30-50 of mixed solution, and the dosage of the sugar-base aqueous corrosive liquid is 3-8 times of the weight of the grid.
8. The positive grid corrosion resistance test method according to claim 1, characterized in that: and 8) drying the positive plate grid by using a vacuum drying box.
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