CN111366852A - In-situ observation method and device for charging state of graphite electrode - Google Patents
In-situ observation method and device for charging state of graphite electrode Download PDFInfo
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- CN111366852A CN111366852A CN202010225749.1A CN202010225749A CN111366852A CN 111366852 A CN111366852 A CN 111366852A CN 202010225749 A CN202010225749 A CN 202010225749A CN 111366852 A CN111366852 A CN 111366852A
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- 239000010439 graphite Substances 0.000 title claims abstract description 43
- 229910002804 graphite Inorganic materials 0.000 title claims abstract description 43
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 42
- 238000011065 in-situ storage Methods 0.000 title claims abstract description 32
- 238000000034 method Methods 0.000 title claims description 23
- 239000010453 quartz Substances 0.000 claims abstract description 22
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 22
- 238000002347 injection Methods 0.000 claims abstract description 9
- 239000007924 injection Substances 0.000 claims abstract description 9
- 239000007788 liquid Substances 0.000 claims abstract description 8
- 239000003792 electrolyte Substances 0.000 claims abstract description 6
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 6
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 6
- 229920002134 Carboxymethyl cellulose Polymers 0.000 claims description 5
- 235000010948 carboxy methyl cellulose Nutrition 0.000 claims description 5
- 229920003048 styrene butadiene rubber Polymers 0.000 claims description 5
- 229910052493 LiFePO4 Inorganic materials 0.000 claims description 4
- 239000011230 binding agent Substances 0.000 claims description 4
- 229910010710 LiFePO Inorganic materials 0.000 claims description 3
- 239000002174 Styrene-butadiene Substances 0.000 claims description 3
- 229910052782 aluminium Inorganic materials 0.000 claims description 3
- 229910052802 copper Inorganic materials 0.000 claims description 3
- 239000010949 copper Substances 0.000 claims description 3
- 239000011889 copper foil Substances 0.000 claims description 3
- 239000011888 foil Substances 0.000 claims description 3
- 229910052759 nickel Inorganic materials 0.000 claims description 3
- 239000012945 sealing adhesive Substances 0.000 claims description 3
- 238000003466 welding Methods 0.000 claims description 3
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 2
- 239000001768 carboxy methyl cellulose Substances 0.000 claims description 2
- 239000008112 carboxymethyl-cellulose Substances 0.000 claims description 2
- 229920006184 cellulose methylcellulose Polymers 0.000 claims description 2
- 239000000203 mixture Substances 0.000 claims description 2
- 239000000565 sealant Substances 0.000 claims description 2
- 210000005069 ears Anatomy 0.000 abstract 3
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 7
- 229910001416 lithium ion Inorganic materials 0.000 description 7
- 230000007547 defect Effects 0.000 description 6
- 238000009830 intercalation Methods 0.000 description 4
- 230000002687 intercalation Effects 0.000 description 4
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 3
- 238000009825 accumulation Methods 0.000 description 3
- 229910052744 lithium Inorganic materials 0.000 description 3
- 238000007789 sealing Methods 0.000 description 3
- FFRBMBIXVSCUFS-UHFFFAOYSA-N 2,4-dinitro-1-naphthol Chemical compound C1=CC=C2C(O)=C([N+]([O-])=O)C=C([N+]([O-])=O)C2=C1 FFRBMBIXVSCUFS-UHFFFAOYSA-N 0.000 description 2
- 229910013465 LiC12 Inorganic materials 0.000 description 2
- 229910013458 LiC6 Inorganic materials 0.000 description 2
- 238000013528 artificial neural network Methods 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 238000009792 diffusion process Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 238000001914 filtration Methods 0.000 description 2
- 238000005259 measurement Methods 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 238000012549 training Methods 0.000 description 2
- 229910013872 LiPF Inorganic materials 0.000 description 1
- 101150058243 Lipf gene Proteins 0.000 description 1
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- 239000002390 adhesive tape Substances 0.000 description 1
- AZDRQVAHHNSJOQ-UHFFFAOYSA-N alumane Chemical compound [AlH3] AZDRQVAHHNSJOQ-UHFFFAOYSA-N 0.000 description 1
- 238000004364 calculation method Methods 0.000 description 1
- 238000004737 colorimetric analysis Methods 0.000 description 1
- 230000001351 cycling effect Effects 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 239000007772 electrode material Substances 0.000 description 1
- 238000004146 energy storage Methods 0.000 description 1
- 230000004927 fusion Effects 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 239000010931 gold Substances 0.000 description 1
- GELKBWJHTRAYNV-UHFFFAOYSA-K lithium iron phosphate Chemical compound [Li+].[Fe+2].[O-]P([O-])([O-])=O GELKBWJHTRAYNV-UHFFFAOYSA-K 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 230000007704 transition Effects 0.000 description 1
Images
Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- 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]
- G01R31/382—Arrangements for monitoring battery or accumulator variables, e.g. SoC
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01J—MEASUREMENT OF INTENSITY, VELOCITY, SPECTRAL CONTENT, POLARISATION, PHASE OR PULSE CHARACTERISTICS OF INFRARED, VISIBLE OR ULTRAVIOLET LIGHT; COLORIMETRY; RADIATION PYROMETRY
- G01J3/00—Spectrometry; Spectrophotometry; Monochromators; Measuring colours
- G01J3/46—Measurement of colour; Colour measuring devices, e.g. colorimeters
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/052—Li-accumulators
- H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/42—Methods or arrangements for servicing or maintenance of secondary cells or secondary half-cells
- H01M10/44—Methods for charging or discharging
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/42—Methods or arrangements for servicing or maintenance of secondary cells or secondary half-cells
- H01M10/48—Accumulators combined with arrangements for measuring, testing or indicating the condition of cells, e.g. the level or density of the electrolyte
- H01M10/488—Cells or batteries combined with indicating means for external visualization of the condition, e.g. by change of colour or of light density
-
- 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
Abstract
The invention discloses an in-situ observation device for the charging state of a graphite electrode, which comprises a quartz box with an opening at the upper end, wherein electrolyte is filled in the quartz box; the working electrodes comprise an anode and a cathode which are tightly attached to the inner wall of the quartz box in parallel edge to edge; the cover plate is provided with two lug leading-out holes and a liquid injection hole; the two pole ear leading-out holes are both provided with pole ears, the lower ends of the two pole ears are respectively and correspondingly connected with the anode and the cathode, and the upper ends of the two pole ears are connected with a power supply. The observation device provided by the invention has the advantages of simple structure, convenience in observation, convenience in calculating results, accuracy and high efficiency.
Description
Technical Field
The invention relates to the field of lithium batteries, in particular to a method and a device for in-situ observation of the charging state of a graphite electrode.
Background
Lithium ion batteries have the advantages of high energy density and long cycle life, and are energy storage devices that are very promising in hybrid vehicles and pure electric vehicles at present and in the future. Graphite is used as an electrode material for many commercial lithium ion batteries because of its high safety, low cost, and stable cycling performance. How to intuitively and simply calculate the real-time SOC of the full battery is very important for studying the performance and the life of the lithium ion battery. Thus, many scholars have performed in-situ observations of graphite electrodes of lithium ion batteries.
The state of charge is an important parameter for describing the chargeable and dischargeable capacity during the use of a battery, and its value is defined as the ratio of the remaining capacity of the battery to the capacity of the battery. At present, the estimation method of the battery SOC mainly includes: discharge experiment method, electric quantity accumulation method, open circuit voltage method, artificial neural network method, Kalman filtering method, etc.
The discharge experiment method has the advantages of reliability and high precision, and has the defects of long time and offline state of the battery during measurement. The charge accumulation method is a simple and reliable estimation method, and has the defect that accumulation errors can be caused due to the current measurement accuracy. The open-circuit voltage method is simple and easy to implement, has higher precision, and has the defect that the battery pack needs to be kept still for a longer time to reach a stable state so as to overcome the self-recovery effect. The Kalman filtering method can not only obtain the estimated value of SOC, but also obtain the estimation error thereof, and has the defects of needing to establish an accurate battery model, large calculation amount and high capability requirement. The artificial neural network method is fast and convenient, has higher precision, can determine the SOC of the battery according to the field working condition, and has the defects that the estimation error is greatly influenced by data and a training method, and a large amount of training data is needed.
At room temperature, the lithium intercalation process of graphite forms a variety of lithium-graphite intercalation compounds: LiC72、LiC36、LiC27、LiC18、LiC12And LiC6. Some lithium-graphite intercalation compounds have a unique color that is distinct from the original gray-black color, such as LiC18、LiC12And LiC6Dark blue, red and gold, respectively.
Therefore, it is an urgent problem to provide a technical means to intuitively and simply calculate the real-time SOC value of the full battery.
Disclosure of Invention
The invention provides a method for in-situ observation of the charging state of a graphite electrode and a device thereof, aiming at solving the defects in the prior art.
In order to achieve the purpose, the invention adopts the following technical scheme:
the first aspect of the present invention provides an in-situ observation apparatus for a charged state of a graphite electrode, comprising:
a quartz box with an opening at the upper end, wherein electrolyte is filled in the quartz box;
the working electrodes comprise an anode and a cathode which are tightly attached to the inner wall of the quartz box in parallel edge to edge; and
a cover plate, on which two polar ear lead-out holes and a liquid injection port are opened; the two pole lug leading-out holes are respectively provided with a pole lug, the lower ends of the two pole lugs are respectively correspondingly connected with the anode and the cathode, and the upper ends of the two pole lugs are connected with a power supply.
Preferably, the upper edges of the four sides of the quartz box extend horizontally outwards to form a box brim, and the cover plate is placed on the box brim.
Preferably, the electrode comprises 90-99% of negative active layer graphite, adhesive, negative current collector copper foil; the electrode comprises a positive active layer LiFePO4And a positive current collector aluminum foil.
Preferably, the binder is a mixture of SBR styrene butadiene rubber and CMC carboxymethyl cellulose.
Preferably, the graphite active layer area of the negative electrode is 1-6mm × 5-10mm, the capacity is 1-3mAh, and the LiFePO of the negative electrode4The active layer area is 1-6mm × 20-40mm, and the capacity is 2-4 mAh.
Preferably, the quartz box is in a rectangular parallelepiped structure.
Preferably, the lithium ion battery also comprises a diaphragm wrapping the positive electrode, wherein the diaphragm is a Celgard2325 three-layer diaphragm, and the thickness of the diaphragm is 20-30 mm.
Preferably, the cover plate is connected with the outer edge of the box eave in a sealing mode through a special sealing adhesive tape; and the two pole lug leading-out holes and the liquid injection port are sealed by using a sealant.
Preferably, the tab connected with the negative electrode is made of copper, and the tab connected with the positive electrode is made of nickel; and the positive electrode, the negative electrode and the lug are welded by using an ultrasonic spot welding machine.
Preferably, the free ends of the positive and negative electrodes are spaced apart by 1-2 mm.
Preferably, the quartz box is in a cuboid structure; the four sides and the bottom surface of the quartz box are fixedly connected in a fusion welding mode.
In a second aspect, the present invention provides an apparatus for a method of in situ observation of the state of charge of a graphite electrode, comprising the steps of:
(1) the in-situ observation device for the charging state of the graphite electrode, which is described in any one of 1-6, is adopted to be connected with a power supply;
(2) capturing a negative electrode image of the in-situ observation device at equal time intervals;
(3) and (3) estimating the real-time SOC value of the negative electrode according to the area of the negative electrode color-changing region relative to the graphite active layer in the negative electrode image obtained in the step (2).
Preferably, the device for capturing the negative electrode image of the in-situ observation device in the step 2 can be a camera, and automatic timing shooting is performed after timing setting is performed on the camera; further preferably, the time interval is 1-3 min.
By adopting the technical scheme, compared with the prior art, the invention has the following technical effects:
the color change of the graphite cathode in the graphite/lithium iron phosphate battery in the lithium intercalation process is observed in real time in a macro-micro manner, the diffusion form of lithium ions in the graphite cathode is analyzed according to the captured in-situ image, and the real-time SOC value of the cathode is further estimated by comparing the area of the cathode color changing region in the cathode image relative to the graphite active layer by using an in-situ colorimetric method.
Drawings
FIG. 1 is a schematic structural diagram of an in-situ observation device for a charged state of a graphite electrode according to the present invention;
FIG. 2 is a schematic diagram of the edge-to-edge arrangement of two electrodes in the present invention;
the reference numerals denote the description:
1-quartz box, 2-cover plate, 3-box eave, 4-liquid injection port, 5-tab lead-out hole, 6-tab and 7-working electrode.
Detailed Description
The present invention will be described in detail and specifically with reference to the following examples to facilitate better understanding of the present invention, but the following examples do not limit the scope of the present invention.
Example 1
The embodiment provides an in-situ observation device for the charging state of a graphite electrode, which comprises a quartz box 1 with an opening at the upper end, and an electrolyte is arranged in the quartz box; the group of working electrodes 7 comprises a positive electrode and a negative electrode, and the edge-to-edge sides are tightly attached to the inner wall of the quartz box 1 in parallel; the cover plate 2 is provided with two tab leading-out holes 5 and a liquid injection port 4; the upper end of the working electrode 7 is fixedly connected with one end of a tab 6, and the other end of the tab 6 extends out of a tab leading-out hole 5 and is connected with a power supply.
In this embodiment, the upper edges of the four sides of the quartz box 1 extend horizontally outward to form a box brim 3, and the cover plate 2 is disposed on the box brim 3.
In the present embodiment, the working electrode 7 includes a positive electrode and a negative electrode; wherein, the negative electrode comprises a negative electrode active layer of 95.7 percent of graphite, a binding agent SBR + CMC and a negative electrode current collector copper foil; the positive electrode comprises a positive active layer LiFePO4Aluminum foil of the positive current collector; further, the diaphragm is Celgard2325 three layersA diaphragm with a thickness of 25mm and 1mol/L LiPF for electrolyte6/(EC+DMC)。
In the embodiment, the area of the graphite active layer of the negative electrode is 4mm × 8mm, the capacity is 1.2672mAh, and the LiFePO of the negative electrode4The active layer area is 4mm × 30mm, and the capacity is 3.264 mAh.
In this embodiment, as shown in fig. 2, the graphite cathode is connected to a copper tab, LiFePO4The anode is connected with the nickel lug; further preferably, the working electrode 7 and the tab 6 are press-connected by an ultrasonic spot welder.
In this embodiment, as shown in FIG. 2, the distance between the free ends of the positive and negative electrodes is 1 to 2 mm.
In this embodiment, the in-situ observation device for the charging state of the graphite electrode needs to be prepared before use, and includes the following steps:
(1) putting the working electrode 7, the quartz box 1 and the cover plate 2 into a vacuum oven, drying for 12 hours at 110 ℃, taking out, putting into a glove box through a transition bin;
(2) two working electrodes 7 are tightly attached to the quartz wall in an edge-to-edge manner, so that the color change of the electrodes can be observed conveniently. Leading the tab 6 to the outside of the device through the tab leading-out hole 5, and sealing the cover plate 2 and the quartz box 1 by using a sealing adhesive tape;
(3) the electrolyte is injected into the device through the injection port 4 at a height higher than the uppermost edge of the electrode. And finally, sealing the liquid injection port by using an adhesive tape.
Example 2
The embodiment provides an in-situ observation method for a charging state of a graphite electrode, which comprises the following steps:
(1) adopting the in-situ observation device for the charging state of the graphite electrode in the embodiment (1), arranging a timing camera at a position where the in-situ observation device can clearly observe the negative electrode, wherein the interval is 2min, connecting the tab with the Shenzhen New Wien battery tester, and setting the charging and discharging multiplying power of the battery tester to be 0.2C;
(2) capturing a negative electrode image of the in-situ observation device every two minutes until the charging is complete;
(3) and (3) estimating the real-time SOC value of the negative electrode according to the size of the area of the graphite active layer (4mm × 8mm) of the golden yellow area of the negative electrode in the negative electrode image obtained in the step (2).
SOC value (area of golden region/area of graphite active layer)
Example 3
In the present example, a method of observing the lithium ion diffusion form from the image obtained in example (2) is provided.
According to the cathode image provided in example (2), a video is formed, and by continuous observation at double speed, it can be clearly observed that the cathode changes from four sides to golden yellow and gradually spreads to the center.
The embodiments of the present invention have been described in detail, but the embodiments are merely examples, and the present invention is not limited to the embodiments described above. Any equivalent modifications and substitutions to those skilled in the art are also within the scope of the present invention. Accordingly, equivalent changes and modifications made without departing from the spirit and scope of the present invention should be covered by the present invention.
Claims (10)
1. An in-situ observation device for the charging state of a graphite electrode, comprising:
a quartz box with an opening at the upper end, wherein electrolyte is filled in the quartz box;
the working electrodes comprise an anode and a cathode which are tightly attached to the inner wall of the quartz box in parallel edge to edge; and
a cover plate, on which two polar ear lead-out holes and a liquid injection port are opened; the two pole lug leading-out holes are respectively provided with a pole lug, the lower ends of the two pole lugs are respectively correspondingly connected with the anode and the cathode, and the upper ends of the two pole lugs are connected with a power supply.
2. The in-situ apparatus for the charging state of a graphite electrode according to claim 1, wherein the quartz box has four upper edges extending horizontally outward from the box to form a box ledge, and the cover plate is disposed on the box ledge.
3. The in-situ apparatus of the state of charge of a graphite electrode of claim 1, wherein the electrode comprises a negative active layer of 90-99% graphite, a binder, a negative current collector copper foil; the electrode comprises a positive active layer LiFePO4 and a positive current collector aluminum foil.
4. The in-situ graphite electrode state of charge device of claim 1, wherein the binder is a mixture of SBR styrene butadiene rubber and CMC carboxymethyl cellulose.
5. The in-situ device for the charging state of the graphite electrode according to claim 2, wherein the graphite active layer area of the negative electrode is 1-6mm × 5-10mm, the capacity is 1-3mAh, and the LiFePO of the negative electrode4The active layer area is 1-6mm × 20-40mm, and the capacity is 2-4 mAh.
6. The in-situ observation device of the charging state of the graphite electrode in claim 1, further comprising a diaphragm wrapping the positive electrode, wherein the diaphragm is a Celgard2325 three-layer diaphragm with a thickness of 20-30 mm.
7. The in-situ observation device of the charging state of the graphite electrode according to claim 2, wherein the cover plate is hermetically connected with the outer edge of the box eave by using a special sealing adhesive tape; and the two pole lug leading-out holes and the liquid injection port are sealed by using a sealant.
8. The in-situ observation device of the charging state of the graphite electrode according to claim 1, wherein the tab connected to the negative electrode is made of copper, and the tab connected to the positive electrode is made of nickel; and the positive electrode and the negative electrode are respectively welded with the lugs by using an ultrasonic spot welding machine.
9. The in-situ observation device of the charging state of the graphite electrode according to claim 1, wherein the distance between the free ends of the positive electrode and the negative electrode is 1-2 mm.
10. A method for in-situ observation of the charging state of a graphite electrode is characterized by comprising the following steps:
(1) the in-situ observation device for the charging state of the graphite electrode, which is described in any one of 1-6, is adopted to be connected with a power supply;
(2) capturing a negative electrode image of the in-situ observation device at equal time intervals;
(3) and (3) estimating the real-time SOC value of the negative electrode according to the area of the negative electrode color-changing region relative to the graphite active layer in the negative electrode image obtained in the step (2).
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112083339A (en) * | 2020-09-13 | 2020-12-15 | 孟*** | Battery charge state monitoring method |
| CN112083339B (en) * | 2020-09-13 | 2024-04-30 | 巨安储能武汉科技有限责任公司 | Battery state of charge monitoring method |
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Application publication date: 20200703 |