CN111307845A - Sampling analysis method for polar plate formation stage - Google Patents
Sampling analysis method for polar plate formation stage Download PDFInfo
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- CN111307845A CN111307845A CN201811592357.8A CN201811592357A CN111307845A CN 111307845 A CN111307845 A CN 111307845A CN 201811592357 A CN201811592357 A CN 201811592357A CN 111307845 A CN111307845 A CN 111307845A
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- 230000015572 biosynthetic process Effects 0.000 title claims abstract description 61
- 238000005070 sampling Methods 0.000 title claims abstract description 39
- 238000004458 analytical method Methods 0.000 title claims abstract description 21
- 239000002253 acid Substances 0.000 claims abstract description 20
- 238000001035 drying Methods 0.000 claims abstract description 9
- 230000020477 pH reduction Effects 0.000 claims abstract description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 12
- 238000003466 welding Methods 0.000 claims description 11
- 229910000679 solder Inorganic materials 0.000 claims description 8
- 239000000835 fiber Substances 0.000 claims description 5
- 238000002791 soaking Methods 0.000 claims description 5
- 239000004698 Polyethylene Substances 0.000 claims description 4
- 238000005192 partition Methods 0.000 claims description 4
- 238000005554 pickling Methods 0.000 claims description 4
- -1 polyethylene Polymers 0.000 claims description 4
- 229920000573 polyethylene Polymers 0.000 claims description 4
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 claims description 3
- 238000005476 soldering Methods 0.000 claims description 3
- 230000010287 polarization Effects 0.000 claims 4
- 230000000694 effects Effects 0.000 abstract description 13
- 238000000034 method Methods 0.000 abstract description 9
- 238000006243 chemical reaction Methods 0.000 abstract description 6
- 238000002441 X-ray diffraction Methods 0.000 description 12
- 239000000126 substance Substances 0.000 description 5
- 230000009286 beneficial effect Effects 0.000 description 3
- 239000003792 electrolyte Substances 0.000 description 3
- 238000001514 detection method Methods 0.000 description 2
- 230000003647 oxidation Effects 0.000 description 2
- 238000007254 oxidation reaction Methods 0.000 description 2
- 238000003487 electrochemical reaction Methods 0.000 description 1
- 238000004146 energy storage Methods 0.000 description 1
- WABPQHHGFIMREM-UHFFFAOYSA-N lead(0) Chemical compound [Pb] WABPQHHGFIMREM-UHFFFAOYSA-N 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
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- G—PHYSICS
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N23/00—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00
- G01N23/20—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by using diffraction of the radiation by the materials, e.g. for investigating crystal structure; by using scattering of the radiation by the materials, e.g. for investigating non-crystalline materials; by using reflection of the radiation by the materials
- G01N23/207—Diffractometry using detectors, e.g. using a probe in a central position and one or more displaceable detectors in circumferential positions
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N23/00—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00
- G01N23/20—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by using diffraction of the radiation by the materials, e.g. for investigating crystal structure; by using scattering of the radiation by the materials, e.g. for investigating non-crystalline materials; by using reflection of the radiation by the materials
- G01N23/20008—Constructional details of analysers, e.g. characterised by X-ray source, detector or optical system; Accessories therefor; Preparing specimens therefor
- G01N23/2005—Preparation of powder samples therefor
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N23/00—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00
- G01N23/22—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by measuring secondary emission from the material
- G01N23/225—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by measuring secondary emission from the material using electron or ion
- G01N23/2251—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by measuring secondary emission from the material using electron or ion using incident electron beams, e.g. scanning electron microscopy [SEM]
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Abstract
The invention provides a sampling analysis method for a polar plate formation stage, which comprises the steps of building a positive and negative polar plate group, acidification formation, sampling at different charging stages, sample drying, XRD testing and SEM testing. The method can comprehensively and objectively analyze the formation condition and the formation effect of the pole plate in each stage in the formation process of the lead-acid storage battery pole plate, and provides technical support for prolonging the service life and the performance of the lead-acid storage battery and researching the reaction mechanism of the pole plate formation.
Description
Technical Field
The invention relates to the technical field of storage batteries, in particular to a sampling analysis method in a pole plate formation stage.
Background
The lead-acid storage battery is widely applied to electric vehicles, electric vehicles and energy storage as a secondary battery, and consists of a positive plate, a negative plate, a partition plate and electrolyte. The lead powder is prepared, a grid is cast, paste is mixed, filling is carried out, curing and drying are carried out, and formation and assembly are carried out. Wherein plate formation of lead-acid batteries is the most critical step in determining battery life and performance. The formation of the electrode plate refers to a process of converting the electrode plate into a positive plate and a negative plate with electrochemical characteristics by using chemical and electrochemical reactions. The formation quality of the lead-acid storage battery plate has more controllable factors, including the pickling time before electrifying, the temperature rise control of the storage battery after injecting the electrolyte, the density of the electrolyte, the formation current and time and the like. At present, no reliable and effective detection and analysis method is available for researching the formation process of the lead-acid storage battery plate. Therefore, a detection and analysis method is needed to evaluate the effect of formation of the lead-acid storage battery plate and the progress of each formation stage, and provide technical support for prolonging the service life and improving the performance of the lead-acid storage battery.
Disclosure of Invention
The invention aims to provide a sampling analysis method for a pole plate formation stage, which can be used for researching and analyzing the progress and formation effect of each stage in the pole plate formation process of a lead-acid storage battery and provides technical support for prolonging the service life and performance of the lead-acid storage battery and researching the reaction mechanism of pole plate formation.
The purpose of the invention is realized by the following technical scheme: a sampling analysis method for a pole plate formation stage comprises the following specific steps:
1) welding a soldering tin wire on each positive plate and each negative plate, wrapping a partition plate outside the positive plates or the negative plates, and arranging the positive plates and the negative plates at intervals; when the positive plate is researched, the positive plate is fewer than the negative plate by one piece; when a negative plate is researched, the negative plate is one less than the positive plate; the minimum number of the positive plates or the negative plates is 5;
2) welding the solder wires on the positive plate together, and welding the solder wires on the negative plate together to form a positive plate group and a negative plate group;
3) carrying out open acidification on the positive and negative electrode plate groups;
4) forming according to the electric quantity 8-12 times of the theoretical capacity of the polar plate, respectively taking 6 samples after standing, pickling, charging by 20%, charging by 40%, charging by 60%, charging by 80% and forming, directly taking down the polar plate to be analyzed during sampling, and simultaneously taking down the polar plate of the other corresponding pole; quickly putting the taken-down polar plate into pure water for soaking;
5) drying the soaked polar plate;
6) taking a test sample on the polar plate, and then carrying out XRD test on the test sample;
7) a test sample was taken from the plate and then SEM-tested on the test sample.
And welding the solder wires on the positive plate and the negative plate, so that the positive plate is conveniently welded to form a positive plate group, the negative plate is welded to form a negative plate group, and finally the positive plate group and the negative plate group are combined to form the positive plate group and the negative plate group. The separator is used for separating two adjacent positive plates from negative plates, so that short circuit caused by direct contact between the positive plates and the negative plates is avoided. The positive and negative plates are formed by open acidification, which is convenient for sampling. In the step 4), sampling is carried out at different charging stages, the taken samples represent formation progress and formation effect of the pole plate at different stages, and the pole plates at different charging stages are respectively sampled and analyzed, so that the formation progress and the formation effect of the pole plate at each stage can be comprehensively analyzed and mastered, and technical support is provided for prolonging the service life and the performance of the lead-acid storage battery and researching the reaction mechanism of pole plate formation. It should be noted that, in each sampling, after the pole plate is taken away, the charging amount needs to be adjusted according to the number of the remaining pole plates, so that the pole plate can reach the set charging state in each sampling. The polar plate sample is taken out and then is quickly put into pure water, so that acid in the polar plate can be removed, and the further oxidation of the polar plate is avoided. The XRD test aims to understand the microstructure of the internal substance of the polar plate at different formation stages, and the formation condition and the formation effect of the polar plate at different stages can be understood through the analysis of the microstructure of the internal substance, so that the XRD test has great significance for the research on the formation mechanism of the polar plate. The SEM test can visually display the structure and the morphology of the surface of the polar plate in different formation stages, and is beneficial to analyzing the formation condition and the formation effect of the polar plate.
Preferably, in step 1), the separator is a polyethylene bag separator. Utilize polyethylene bag formula baffle parcel outside positive plate or negative plate, compare traditional piece formula polar plate, be difficult for droing, be fit for using under experimental analysis condition.
Preferably, in step 3), the density of the acid is 0.8-1.3g/cm3 when the open acidification is carried out.
Preferably, in the step 4), the electrode plate is soaked in the pure water for 12-24 hours, and the pure water is replaced every 2-4 hours. The polar plate is soaked for 12-24 hours, and pure water is replaced at regular time in the soaking process, so that acid in the polar plate can be effectively removed.
Preferably, in the step 5), the temperature at the time of drying is 30 to 55 ℃ and the drying time is 24 to 48 hours.
Preferably, in step 6), sampling is performed at 9 positions of the plate, namely, the upper, middle, lower, left, middle and right positions, the removed test samples are numbered from 1 to 9, the removed test samples are ground, short fibers in the ground test samples are screened out, and then XRD (X-ray diffraction) test is performed. The test samples are taken from the upper, middle, lower, left, middle and right positions of the polar plate, so that the internal microstructure of each part of the polar plate can be comprehensively and objectively analyzed, and the formation condition and the formation effect of each part of the polar plate can be comprehensively known. Short fibers in a test sample are screened out, so that the influence of the short fibers on an XRD test result is avoided.
Preferably, in step 6), the XRD test is carried out with a scanning angle of 10-90 degrees.
Preferably, in the step 7), when a test sample is taken, taking 9 positions of the upper part, the middle part, the lower part, the left part, the middle part and the right part of the polar plate as sampling positions, respectively taking out a single lattice of lead paste at each sampling position, and numbering the taken sample by 1-9; when SEM test is carried out, cross section observation is carried out on one side of the test sample close to the grid ribs and the middle of the test sample, and point taking observation is carried out between the edge of the cross section and the center of the cross section during observation. The surface structure and the appearance of each part of the cross section on the polar plate can be comprehensively and objectively analyzed by taking test samples from 9 positions of the polar plate, namely the upper position, the middle position, the lower position, the left position, the middle position and the right position. By observing points from the edge of the cross section to the center of the cross section, the structural condition of each point of the test sample from outside to inside and the change process of the test sample from outside to inside can be mastered, so that the test result is more comprehensive and reliable.
Preferably, the observation magnification is 1000 times, 3000 times, 5000 times, 7000 times, and 1 ten thousand times when the SEM test is performed.
The invention has the beneficial effects that: the method can comprehensively and objectively analyze the formation condition and the formation effect of the pole plate in each stage in the formation process of the lead-acid storage battery pole plate, and provides technical support for prolonging the service life and the performance of the lead-acid storage battery and researching the reaction mechanism of the pole plate formation.
Drawings
FIG. 1 is a schematic view of a test sample in the present invention at a sampling position on a pad.
Detailed Description
The invention is further described by the following detailed description in conjunction with the accompanying drawings.
Example (b): a sampling analysis method for a pole plate formation stage comprises the following specific steps:
1) welding a soldering tin wire on each positive plate and each negative plate, wrapping a partition plate outside the positive plates or the negative plates, and arranging the positive plates and the negative plates at intervals; when the positive plate is researched, the positive plate is one piece less than the negative plate, and when the negative plate is researched, the negative plate is one piece less than the positive plate; the minimum number of positive or negative plates is 5. The clapboard is a polyethylene bag type clapboard.
2) And welding the solder wires on the positive plate together, and welding the solder wires on the negative plate together to form a positive plate group and a negative plate group.
3) And (3) carrying out open acidification formation on the positive and negative electrode plate groups, wherein the density of the acid is 0.8-1.3g/cm 3.
4) Forming according to the electric quantity 8-12 times of the theoretical capacity of the polar plate, respectively taking 6 samples after standing, pickling, charging by 20%, charging by 40%, charging by 60%, charging by 80% and forming, directly taking down the polar plate to be analyzed during sampling, and simultaneously taking down the polar plate of the other corresponding pole; and quickly putting the taken-down polar plate into pure water for soaking. The time for soaking the polar plate in the pure water is 12-24 hours, and the pure water is replaced every 2-4 hours.
5) Drying the soaked polar plate at 30-55 deg.C for 24-48 hr.
6) A test sample is taken on the polar plate, and then the XRD test is carried out on the test sample. When a test sample is taken, sampling is respectively carried out at 9 positions of the upper part, the middle part, the lower part, the left part, the middle part and the right part of the polar plate (the specific sampling position is shown in figure 1), the number of 1-9 is carried out on the taken test sample, the taken test sample is ground, short fibers in the taken test sample are screened out, and then XRD test is carried out. When XRD test is carried out, the scanning angle is 10-90 degrees.
7) A test sample was taken from the plate and then SEM-tested on the test sample. When a test sample is taken, 9 positions of the upper part, the middle part, the lower part, the left part, the middle part and the right part of the polar plate are taken as sampling positions (the specific sampling positions are shown in figure 1), a single lattice of lead paste is taken out from each sampling position, and the number of the taken-down sample is 1-9. When SEM test is carried out, cross section observation is carried out on one side of the test sample close to the grid ribs and the middle of the test sample, and point taking observation is carried out between the edge of the cross section and the center of the cross section during observation. For SEM test, the magnification of observation was selected to be 1000 times, 3000 times, 5000 times, 7000 times and 1 ten thousand times.
And welding the solder wires on the positive plate and the negative plate, so that the positive plate is conveniently welded to form a positive plate group, the negative plate is welded to form a negative plate group, and finally the positive plate group and the negative plate group are combined to form the positive plate group and the negative plate group. The separator is used for separating two adjacent positive plates from negative plates, so that short circuit caused by direct contact between the positive plates and the negative plates is avoided. The positive and negative plates are formed by open acidification, which is convenient for sampling. In the step 4), sampling is carried out at different charging stages, the taken samples represent formation progress and formation effect of the pole plate at different stages, and the pole plates at different charging stages are respectively sampled and analyzed, so that the formation progress and the formation effect of the pole plate at each stage can be comprehensively analyzed and mastered, and technical support is provided for prolonging the service life and the performance of the lead-acid storage battery and researching the reaction mechanism of pole plate formation. It should be noted that, in each sampling, after the pole plate is taken away, the charging amount needs to be adjusted according to the number of the remaining pole plates, so that the pole plate can reach the set charging state in each sampling. The polar plate sample is taken out and then is quickly put into pure water, so that acid in the polar plate can be removed, and the further oxidation of the polar plate is avoided. The XRD test aims to understand the microstructure of the internal substance of the polar plate at different formation stages, and the formation condition and the formation effect of the polar plate at different stages can be understood through the analysis of the microstructure of the internal substance, so that the XRD test has great significance for the research on the formation mechanism of the polar plate. The SEM test can visually display the structure and the morphology of the surface of the polar plate in different formation stages, and is beneficial to analyzing the formation condition and the formation effect of the polar plate.
Finally, it should be noted that: although the present invention has been described in detail with reference to the foregoing embodiments, it will be apparent to those skilled in the art that modifications may be made to the embodiments or portions thereof without departing from the spirit and scope of the invention.
Claims (9)
1. A sampling analysis method for a pole plate formation stage is characterized by comprising the following specific steps:
1) welding a soldering tin wire on each positive plate and each negative plate, wrapping a partition plate outside the positive plates or the negative plates, and arranging the positive plates and the negative plates at intervals; when the positive plate is researched, the positive plate is one less than the negative plate; when a negative plate is researched, the negative plate is one less than the positive plate; the minimum number of the positive plates or the negative plates is 5;
2) welding the solder wires on the positive plate together, and welding the solder wires on the negative plate together to form a positive plate group and a negative plate group;
3) carrying out open acidification on the positive and negative electrode plate groups;
4) forming according to the electric quantity 8-12 times of the theoretical capacity of the polar plate, respectively taking 6 samples after standing, pickling, charging by 20%, charging by 40%, charging by 60%, charging by 80% and forming, directly taking down the polar plate to be analyzed during sampling, and simultaneously taking down the polar plate of the other corresponding pole; quickly putting the taken-down polar plate into pure water for soaking;
5) drying the soaked polar plate;
6) taking a test sample on the polar plate, and then carrying out XRD test on the test sample;
7) a test sample was taken from the plate and then SEM-tested on the test sample.
2. A sampling analysis method in a plate polarization stage according to claim 1, wherein in step 1), the separator is a polyethylene bag separator.
3. A sampling analysis method in a plate polarization stage according to claim 1, wherein in step 3), the density of the acid is 0.8-1.3g/cm3 when the open-top acidification is performed.
4. The sampling analysis method for the pole plate formation stage according to claim 1, wherein in the step 4), the pole plate is soaked in pure water for 12-24 hours, and the pure water is replaced every 2-4 hours.
5. A sampling analysis method for a plate formation stage according to claim 1, wherein in the step 5), the temperature for drying is 30-55 ℃ and the drying time is 24-48 hours.
6. A sampling analysis method for a pole plate formation stage according to claim 1, 2, 3, 4 or 5, characterized in that in step 6), when a test sample is taken, the test sample is respectively sampled at 9 positions of the pole plate, namely, the upper, middle, lower, left, middle and right positions, the number of the taken test sample is 1-9, the taken test sample is ground and short fibers are screened out, and then the XRD test is carried out.
7. A sampling analysis method for a polarization plate formation stage according to claim 6, wherein in the step 6), when XRD test is performed, the scanning angle is 10-90 degrees.
8. A sampling analysis method in a pole plate formation stage according to claim 1, 2, 3, 4 or 5, wherein in the step 7), when a test sample is taken, 9 positions of the pole plate, namely the upper, middle, lower, left, middle and right positions, are taken as sampling positions, a single lattice of lead paste is taken out at each sampling position, and the taken-out sample is numbered from 1 to 9; when SEM test is carried out, cross section observation is carried out on one side of the test sample close to the grid ribs and the middle of the test sample, and point taking observation is carried out between the edge of the cross section and the center of the cross section during observation.
9. A sampling analysis method in a plate polarization formation stage according to claim 8, wherein the observation magnification is 1000 times, 3000 times, 5000 times, 7000 times and 1 ten thousand times when SEM test is performed.
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| CN201811592357.8A CN111307845A (en) | 2018-12-25 | 2018-12-25 | Sampling analysis method for polar plate formation stage |
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101101998A (en) * | 2006-07-06 | 2008-01-09 | 夏振明 | High-capacity and long-life metal silk weaved light bar lead acid battery for electric motorcar |
| CN107621453A (en) * | 2017-10-11 | 2018-01-23 | 超威电源有限公司 | The detection method of lead ion content in a kind of power type lead accumulator dividing plate |
| CN108088698A (en) * | 2017-11-03 | 2018-05-29 | 超威电源有限公司 | A kind of pole plate sampling and analyzing method of cure stage |
| CN108183239A (en) * | 2017-12-29 | 2018-06-19 | 骆驼集团襄阳蓄电池有限公司 | A kind of AGM start-stops negative electrode grid surface treatment method |
-
2018
- 2018-12-25 CN CN201811592357.8A patent/CN111307845A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101101998A (en) * | 2006-07-06 | 2008-01-09 | 夏振明 | High-capacity and long-life metal silk weaved light bar lead acid battery for electric motorcar |
| CN107621453A (en) * | 2017-10-11 | 2018-01-23 | 超威电源有限公司 | The detection method of lead ion content in a kind of power type lead accumulator dividing plate |
| CN108088698A (en) * | 2017-11-03 | 2018-05-29 | 超威电源有限公司 | A kind of pole plate sampling and analyzing method of cure stage |
| CN108183239A (en) * | 2017-12-29 | 2018-06-19 | 骆驼集团襄阳蓄电池有限公司 | A kind of AGM start-stops negative electrode grid surface treatment method |
Non-Patent Citations (2)
| Title |
|---|
| L. PROUT: "Aspects of lead/acid battery technology 4. Plate formation", 《JOURNAL OF POWER SOURCES》 * |
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