CN111769255A - Positive pole piece for high-power lithium-manganese dioxide battery and preparation method thereof - Google Patents
Positive pole piece for high-power lithium-manganese dioxide battery and preparation method thereof Download PDFInfo
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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
- H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
- H01M4/134—Electrodes based on metals, Si or alloys
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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
- H01M4/04—Processes of manufacture in general
- H01M4/0402—Methods of deposition of the material
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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
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- H01M4/043—Processes of manufacture in general involving compressing or compaction
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- H—ELECTRICITY
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- 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
- H01M4/04—Processes of manufacture in general
- H01M4/0471—Processes of manufacture in general involving thermal treatment, e.g. firing, sintering, backing particulate active material, thermal decomposition, pyrolysis
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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
- H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
- H01M4/131—Electrodes based on mixed oxides or hydroxides, or on mixtures of oxides or hydroxides, e.g. LiCoOx
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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
- H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
- H01M4/139—Processes of manufacture
- H01M4/1391—Processes of manufacture of electrodes based on mixed oxides or hydroxides, or on mixtures of oxides or hydroxides, e.g. LiCoOx
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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
- H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
- H01M4/139—Processes of manufacture
- H01M4/1395—Processes of manufacture of electrodes based on metals, Si or alloys
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- 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
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Abstract
The invention discloses a positive pole piece for a high-power lithium-manganese dioxide battery and a preparation method thereof, the method comprises the steps of carrying out heat treatment on electrolytic manganese dioxide serving as an active substance, mixing the electrolytic manganese dioxide with a conductive agent and a binding agent, grinding, heating and drying, adding N-methyl pyrrolidone, stirring and mixing to obtain a positive pole mixture; and (3) uniformly coating the positive electrode mixture on the surface of the current collector by using a coating machine, drying, and pressing to 0.1-0.3 mm by using a roller press to obtain the positive electrode plate for the high-power lithium-manganese dioxide battery. The method has simple process, can greatly improve the capacity characteristic and the large-current pulse discharge performance of the lithium-manganese dioxide battery by controlling the thickness and the porosity of the electrode, and meets the requirement of the high-power manganese dioxide battery.
Description
Technical Field
The invention relates to the technical field of lithium batteries, in particular to a positive pole piece for a high-power lithium-manganese dioxide battery and a preparation method thereof.
Background
A lithium-manganese dioxide battery belongs to a lithium primary battery and is prepared by taking metal lithium as a negative electrode, taking solid salt or salt dissolved in an organic solvent as an electrolyte and taking electrolytic manganese dioxide after heat treatment as a positive electrode. The device has wide application range and is mainly used for power supplies of electronic calculators, radios, flashlights, electric toys, watches, survival equipment, intelligent water meters, positioning emitters and instrument memory equipment.
With the gradual popularization of the internet of things technology, the battery requirements matched with the internet of things chip or terminal are increasing. Different from traditional electrical apparatus, the thing networking device is applied to response, wireless connection scene mostly, need support the signal at any time and in the equipment quick connection, requires the battery to have concurrently resistant storage and connect instantaneous heavy current pulse discharge ability, and at present, lithium primary battery will be the main power supply mode at thing networking chip and terminal.
Most of conventional button-type lithium-manganese dioxide batteries adopt a sheet pressing method or a paste coating method to prepare a positive pole piece, the prepared positive pole piece is thick and about 2mm, and can meet the requirement of long-time minimum current discharge, but the battery voltage drop is increased when the battery discharges with large current due to the fact that the pole piece is too thick, the porosity is too low, the ohmic polarization is large, and the mass transfer characteristic of lithium ions is poor, so that the voltage output is influenced, and the battery cannot be applied to the scene of large-current pulse discharge.
Disclosure of Invention
One object of the present invention is: the positive pole piece for the lithium-manganese dioxide battery and the preparation method thereof are provided, can meet the requirement of large-current pulse discharge, and simultaneously improve the utilization rate of positive active substances and the capacity characteristic of the battery.
In order to achieve the purpose, the invention adopts the following technical scheme:
a preparation method of a positive pole piece for a lithium-manganese dioxide battery comprises the following steps:
(1) mixing heat-treated electrolytic manganese dioxide powder serving as an active material with a conductive agent and a binder, and grinding to obtain a grinding mixture;
(2) drying the ground mixture to obtain a positive electrode mixture;
(3) adding N-methyl pyrrolidone serving as a solvent into the positive electrode mixture, fully mixing and stirring to prepare positive electrode slurry;
(4) uniformly coating the positive slurry on an aluminum foil serving as a current collector by using a coating machine, and drying in a vacuum drying oven;
(5) and (3) thinning the positive pole piece by using a roller press to obtain the positive pole piece for the high-power lithium-manganese dioxide battery.
The preparation method is suitable for preparing the positive pole piece for the button and soft package lithium-manganese dioxide battery.
The further technical scheme is that the grinding mixture in the step (1) is mainly prepared from the following raw materials in percentage by mass:
manganese dioxide: 80 to 96 percent
Conductive agent: 2 to 10 percent
Adhesive: 2 to 10 percent
The sum of the mass percent of the raw materials is 100 percent
The further technical scheme is that the conductive agent is selected from any one or a combination of at least two of graphite, conductive carbon black, acetylene black, carbon nanotubes or graphene, and is further preferably a combination of graphite and conductive carbon black, wherein the mass ratio of the graphite to the conductive carbon black is 1: 1.
The further technical scheme is that the binder is selected from one or a combination of at least two of polyvinylidene fluoride, polyacrylate or polyacrylonitrile, and is further preferably polyvinylidene fluoride.
The further technical scheme is that the drying temperature in the step (2) is 50-90 ℃, such as 50 ℃, 55 ℃, 60 ℃, 65 ℃, 70 ℃, 75 ℃, 80 ℃, 85 ℃, 90 ℃ and the like, but not limited to the enumerated values, other unrecited values in the above numerical ranges are also used, and the further optimized temperature is 60-70 ℃.
The further technical scheme is that the drying time in the step (2) is 2-5 h, such as 2h, 2.5h, 3h, 3.5h, 4h, 4.5h or 5h, but is not limited to the enumerated values, and other unrecited values in the above numerical ranges are also used, and further preferably 2-3 h.
In a further technical solution, the solid content of the positive electrode slurry in the step (3) is 35% to 60%, such as 35%, 40%, 45%, 50%, 55%, 60%, etc., but the solid content is not limited to the recited values, and other unrecited values within the above numerical ranges are also used, and more preferably 45% to 50%.
The further technical scheme is that the drying temperature in the step (4) is 100-160 ℃, such as 100 ℃, 110 ℃, 120 ℃, 130 ℃, 140 ℃, 160 ℃, but not limited to the recited values, and other unrecited values in the above numerical ranges are also used, and more preferably 110-130 ℃.
According to a further technical scheme, in the step (4), the drying time is 9-15 hours, such as 9 hours, 10 hours, 11 hours, 12 hours, 13 hours, 14 hours, 15 hours and the like, but the drying time is not limited to the enumerated values, other unrecited values in the above numerical ranges are also used, and the drying time is more preferably 10-12 hours.
Further, in the step (5), the rolling thickness is 80 to 300 μm, such as 80 μm, 100 μm, 120 μm, 140 μm, 160 μm, 180 μm, 200 μm, 220 μm, 240 μm, 260 μm, 280 μm, 300 μm, but is not limited to the above-mentioned values, and other values not listed in the above-mentioned value ranges are used in the same manner, and more preferably 180 to 220 μm.
The invention also provides the positive pole piece for the lithium-manganese dioxide battery, which is prepared by the preparation method.
Compared with the prior art, the invention has the following beneficial effects:
(1) the preparation method provided by the invention optimizes the mixing and homogenizing processes. In the prior art, the active substance is usually mixed with the conductive agent, and then the binder emulsion is added for homogenization. At higher solids content, the binder proportion in the binder emulsion is too high, resulting in a higher emulsion viscosity, difficulty in thorough mixing during homogenization, and possibly leading to coating failure of the slurry.
The method is optimized and improved aiming at the problems, the active substance, the conductive agent and the binder powder are fully mixed before homogenizing, the particle agglomeration phenomenon can be effectively reduced, the dry materials are fully mixed, the formation of a pole piece conductive network is promoted during homogenizing, and the adhesion of the pole piece is improved; meanwhile, the positive electrode mixture is dried, so that impurities such as water, polyvinyl alcohol and the like contained in the positive electrode active material electrolytic manganese dioxide can be effectively removed; in addition, according to the method, all dry materials are fully mixed, and then N-methyl pyrrolidone serving as a solvent or a dispersing agent is added, so that the solid content of the anode slurry is more controllable, the solid content can be increased, the fluidity of the slurry can be ensured, and a thicker pole piece can be prepared by adopting a coating method.
(2) According to the preparation method provided by the invention, the solid content and the thickness of the pole piece are controlled, so that the prepared pole piece has excellent high-current discharge performance while keeping high compaction density, and the compaction density can reach 2.7-2.8 g/cm3. The power supply device can be applied to power supply of chips or terminals of the Internet of things, and meets the requirement of pulse discharge.
(3) The preparation method provided by the invention has simple process, does not need to adjust the existing production process device, and is beneficial to industrial production.
Detailed Description
In order to better illustrate the present invention and to facilitate an understanding of the technical solutions of the present invention, the present invention is further described in detail below. The following examples are merely illustrative of the present invention and do not represent or limit the scope of the claims, which are defined by the claims.
The following are typical but non-limiting examples of the invention:
example 1
A preparation method of a positive pole piece for a lithium-manganese dioxide battery comprises the following steps:
mixing and grinding 80% of electrolytic manganese dioxide, 5% of graphite, 5% of conductive carbon black and 10% of polyvinylidene fluoride, and drying for 2 hours; adding N-methyl pyrrolidone into the mixed powder, and fully mixing to prepare anode slurry with the solid content of 36%; coating the positive electrode slurry on a coating machine and drying the positive electrode slurry for 12 hours in vacuum at 110 ℃; rolling the dried pole piece into a pole piece with the thickness of 110 mu m by using a rolling machine to obtain a lithium-manganese dioxide battery positive pole piece;
example 2
A preparation method of a positive pole piece for a lithium-manganese dioxide battery comprises the following steps:
mixing and grinding 80% of electrolytic manganese dioxide, 5% of graphite, 5% of conductive carbon black and 10% of polyvinylidene fluoride, and drying for 2 hours; adding N-methyl pyrrolidone into the mixed powder, and fully mixing to prepare anode slurry with the solid content of 40%; coating the positive electrode slurry on a coating machine and drying the positive electrode slurry for 12 hours in vacuum at 110 ℃; rolling the dried pole piece into a pole piece with the thickness of 150 mu m by using a rolling machine to obtain a lithium-manganese dioxide battery positive pole piece;
example 3
A preparation method of a positive pole piece for a lithium-manganese dioxide battery comprises the following steps:
mixing and grinding 80% of electrolytic manganese dioxide, 5% of graphite, 5% of conductive carbon black and 10% of polyvinylidene fluoride, and drying for 2 hours; adding N-methyl pyrrolidone into the mixed powder, and fully mixing to prepare anode slurry with the solid content of 40%; coating the positive slurry on a coating machine and drying the positive slurry for 12 hours in vacuum at 120 ℃; rolling the dried pole piece into a pole piece with the thickness of 190 mu m by using a rolling machine to obtain a lithium-manganese dioxide battery positive pole piece;
example 4
A preparation method of a positive pole piece for a lithium-manganese dioxide battery comprises the following steps:
mixing and grinding 90% of electrolytic manganese dioxide, 2.5% of graphite, 2.5% of conductive carbon black and 5% of polyvinylidene fluoride, and drying for 2 hours; adding N-methyl pyrrolidone into the mixed powder, and fully mixing to prepare anode slurry with solid content of 48%; coating the positive slurry on a coating machine and drying the positive slurry for 15 hours in vacuum at 120 ℃; rolling the dried pole piece into a pole piece with the thickness of 200 mu m by using a rolling machine to obtain a lithium-manganese dioxide battery positive pole piece;
example 5
A preparation method of a positive pole piece for a lithium-manganese dioxide battery comprises the following steps:
mixing and grinding 90% of electrolytic manganese dioxide, 2.5% of graphite, 2.5% of conductive carbon black and 5% of polyvinylidene fluoride, and drying for 2 hours; adding N-methyl pyrrolidone into the mixed powder, and fully mixing to prepare anode slurry with solid content of 50%; coating the positive slurry on a coating machine and drying the positive slurry for 10 hours in vacuum at 110 ℃; rolling the dried pole piece into a pole piece with the thickness of 250 mu m by using a rolling machine to obtain a lithium-manganese dioxide battery positive pole piece;
example 6
A preparation method of a positive pole piece for a lithium-manganese dioxide battery comprises the following steps:
mixing and grinding 92% of electrolytic manganese dioxide, 2% of graphite, 2% of conductive carbon black and 4% of polyvinylidene fluoride, and drying for 2 hours; adding N-methyl pyrrolidone into the mixed powder, and fully mixing to prepare anode slurry with solid content of 48%; coating the positive electrode slurry on a coating machine and drying the positive electrode slurry for 11 hours in vacuum at 110 ℃; rolling the dried pole piece into a pole piece with the thickness of 200 mu m by using a rolling machine to obtain a lithium-manganese dioxide battery positive pole piece;
comparative example 1
The preparation method of the pole piece of the comparative example comprises the following steps:
fully grinding and mixing 90% of electrolytic manganese dioxide, 2.5% of graphite and 2.5% of conductive carbon black, drying for 2 hours, fully mixing with a polytetrafluoroethylene binder (the mass percentage of polytetrafluoroethylene is 5%), pressing into a pole piece by using a powder tablet press, and drying in vacuum at 160 ℃ for 12 hours. Preparing the positive pole piece with the thickness of 1 mm.
Test method
The positive electrode plates prepared in the above examples 1 to 6 and comparative example 1 were used as the positive electrode of the cell, and the CR2032 type button cell was assembled with metal lithium as the negative electrode, electrolyte (1mol/L solution of propylene carbonate/ethylene glycol dimethyl ether (volume ratio 1:1) of lithium perchlorate), and polypropylene separator.
And carrying out constant current discharge test and pulse discharge test on the assembled battery.
The discharge current of the constant current discharge test is 2.5mA/g and 12.5mA/g, and the discharge cut-off voltage is 1V.
The pulse discharge conditions are respectively set as 250mAh/g, 500mAh/g and 750mAh/g, the pulse discharge time is 10s, then the mixture is stood for 1h, the pulse discharge is carried out for 5 times, and the battery voltage at the end of the pulse discharge is recorded.
The constant current discharge data are shown in table 1.
Table 1 constant current discharge data
| Numbering | 2.5mA/g discharge time/h | 12.5mA/g discharge time/h |
| Example 1 | 108 | 19 |
| Example 2 | 132 | 20.2 |
| Example 3 | 120 | 18.9 |
| Example 4 | 101 | 17.5 |
| Example 5 | 99 | 18 |
| Example 6 | 100 | 18.5 |
| Comparative example 1 | 70 | 6 |
The pulse discharge data are shown in table 2.
TABLE 2 pulse discharge data
Combining the test results of the above examples and comparative examples, it can be seen that examples 1-6 prepared by the present invention have excellent capacity characteristics, and the low current discharge capacity far exceeds that of the pole piece prepared by the sheet pressing method (comparative example 1). Meanwhile, the material shows excellent pulse discharge characteristics, and can complete pulse discharge at about 3C multiplying power. While comparative example 1, which was prepared by the tablet press method, was completely incapable of performing pulse discharge.
The preparation method of the positive pole piece provided by the invention has excellent capacity characteristic and pulse discharge performance, and the power characteristic is more excellent. The pole piece is prepared by a coating method, so that the active substance, the conductive agent and the binder are mixed more uniformly, the conductivity of the pole piece is enhanced, and the ohmic resistance is reduced; through adjusting pole piece thickness and porosity, strengthen the mass transfer characteristic of lithium ion in electrolyte, reduce concentration polarization, promote the discharge voltage platform, improve the active material utilization ratio, possess excellent heavy current pulse discharge characteristic simultaneously.
Although the present invention has been described herein with reference to the illustrated embodiments thereof, which are intended to be preferred embodiments of the present invention, it is to be understood that the invention is not limited thereto, and that numerous other modifications and embodiments can be devised by those skilled in the art that will fall within the spirit and scope of the principles of this disclosure.
Claims (9)
1. A preparation method of a positive pole piece for a high-power lithium-manganese dioxide battery is characterized by comprising the following steps:
(1) mixing heat-treated electrolytic manganese dioxide powder serving as an active material with a conductive agent and a binder, and grinding to obtain a grinding mixture;
(2) drying the ground mixture to obtain a positive electrode mixture;
(3) adding N-methyl pyrrolidone serving as a solvent into the positive electrode mixture, fully mixing and stirring to prepare positive electrode slurry;
(4) uniformly coating the positive slurry on an aluminum foil serving as a current collector by using a coating machine, and drying in a vacuum drying oven;
(5) and (3) thinning the positive pole piece by using a roller press to obtain the positive pole piece for the high-power lithium-manganese dioxide battery.
2. The preparation method of the positive pole piece for the high-power lithium-manganese dioxide battery according to claim 1, wherein the active material is 80-96 wt%, the conductive agent is 2-10 wt%, the binder is 2-10 wt%, and the sum of the active material, the conductive agent and the binder is 100 wt%.
3. The preparation method of the positive pole piece for the high-power lithium-manganese dioxide battery as claimed in claim 1, wherein the conductive agent is one or more selected from carbon black, acetylene black, carbon nanotubes and graphene, and the binder is one or more selected from polyvinylidene fluoride, polyacrylate and polyacrylonitrile.
4. The method for preparing the positive pole piece of the high-power lithium-manganese dioxide battery according to claim 1, wherein the drying temperature of the grinding mixture in the step (2) is 50-90 ℃.
5. The preparation method of the positive pole piece for the high-power lithium-manganese dioxide battery according to claim 1, wherein the drying time of the ground mixture in the step (2) is 2-5 h.
6. The method for preparing the positive pole piece for the high-power lithium-manganese dioxide battery according to claim 1, wherein the solid content in the positive pole mixture obtained in the step (2) is 30-60%.
7. The preparation method of the positive pole piece for the high-power lithium-manganese dioxide battery according to claim 1, wherein the drying temperature in the step (4) is 110-160 ℃, and the drying time is 9-15 hours.
8. The preparation method of the positive pole piece for the high-power lithium-manganese dioxide battery according to claim 1, wherein the rolled thickness of the positive pole piece in the step (5) is 80-300 μm.
9. A positive pole piece for a high-power lithium-manganese dioxide battery is characterized by being prepared by the preparation method of any one of claims 1-8.
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| CN113517441A (en) * | 2021-03-31 | 2021-10-19 | 广西大学 | Method for modifying lithium manganese battery by graphene |
| CN114883517A (en) * | 2022-06-07 | 2022-08-09 | 江门市宏力能源有限公司 | Preparation method of battery pole piece for improving large-current discharge capacity |
| WO2023102778A1 (en) * | 2021-12-08 | 2023-06-15 | Medtrum Technologies Inc. | Positive electrode plate for medical device battery and its preparation method |
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| CN112670451A (en) * | 2020-12-29 | 2021-04-16 | 西北工业大学 | Preparation method of organic composite positive electrode for improving energy density of lithium-manganese battery for underwater vehicle |
| CN112670451B (en) * | 2020-12-29 | 2022-11-11 | 西北工业大学 | Preparation method of organic composite positive electrode for improving energy density of lithium-manganese battery for underwater vehicle |
| CN113517441A (en) * | 2021-03-31 | 2021-10-19 | 广西大学 | Method for modifying lithium manganese battery by graphene |
| WO2023102778A1 (en) * | 2021-12-08 | 2023-06-15 | Medtrum Technologies Inc. | Positive electrode plate for medical device battery and its preparation method |
| CN114883517A (en) * | 2022-06-07 | 2022-08-09 | 江门市宏力能源有限公司 | Preparation method of battery pole piece for improving large-current discharge capacity |
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