CN109698318B - Based on MnO2Positive plate of lithium ion battery of PEDOT and preparation method - Google Patents
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Abstract
Based on MnO2-positive plate of PEDOT lithium ion battery, comprising positive plate, nano MnO formed on the positive plate by electrochemical method2Thin film in MnO2PEDOT film formed on the film and uniformly coated on MnO2Positive electrode paste on the film; the positive electrode slurry comprises a positive electrode active material, a gel-like adhesive and a conductive agent; the gel-like adhesive is a high-molecular conductive polymer formed by polymerizing monomers. The MnO 2-PEDOT-based lithium ion battery has the advantages of high specific capacity of the positive plate, high conductivity and good cycling stability.
Description
Technical Field
The invention relates to a lithium ion battery, in particular to a MnO2-PEDOT based positive plate of the lithium ion battery and a preparation method thereof.
Background
Lithium ion batteries have the advantages of high energy density, high power density, short charging time, long service life, high cycle efficiency and the like, and are increasingly paid more attention by people. The acquisition of high specific volume electrode materials is a research hotspot of lithium ion batteries. The conductive polymer poly-3, 4-ethylenedioxythiophene (PEDOT) has the advantages of high specific volume, high conductivity, good thermal stability and the like, and is an ideal electrode material of the lithium ion battery, but the PEDOT material has poor mechanical stability, so that the cycle life of the PEDOT material is poor, and the PEDOT material becomes the biggest obstacle for preventing the application of the PEDOT electrode film in the lithium ion battery.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provides a positive plate of a lithium ion battery based on MnO2-PEDOT, which has high specific capacity, high conductivity and good cycling stability, and a preparation method thereof.
In order to solve the technical problems, the technical scheme provided by the invention is as follows: based on MnO2-positive plate of PEDOT lithium ion battery, comprising positive plate, nano MnO formed on the positive plate by electrochemical method2Thin film in MnO2PEDOT film formed on the film and uniformly coated on MnO2Positive electrode paste on the film; the positive electrode slurry comprises a positive electrode active material, a gel-like adhesive and a conductive agent; the gel-like adhesive is a high-molecular conductive polymer formed by polymerizing monomers. As shown in FIG. 1(a) and FIG. 1(b), in the present invention, cyclic voltammetry is used to deposit MnO on a positive electrode sheet2So that MnO is formed2The film is composed of numerous irregular MnO2The nano particles are mutually interlaced and stacked, and have larger comparative area when in MnO2When growing PEDOT on thin films, PEDOT will first accumulate in the MnO2MnO formed by nano particles2Surface of the nanosheet, MnO2The nanosheets are wrapped, and as the reaction further progresses, PEDOT can completely cover MnO2The thin film is formed, and a PEDOT thin film layer with a plurality of micropores is formed on the thin film, so that the MnO2-PEDOT composite thin film formed on the positive plate has larger surface area. In the present invention, MnO2The particles play a role of mechanical support for PEDOT material, and the PEDOT material is attached to MnO when being charged and discharged2The PEDOT on the surface of the nanosheet cannot deform irreversibly, and the composite electrode has good cycle characteristics. In the present invention, the positive electrode slurry is coated on MnO2Since the adhesion between organic materials is much better than that between an organic material and an inorganic material, the PEDOT composite film is positive in charge-discharge cyclesThe electrode slurry is not easy to fall off from the positive plate, cracks are not easy to generate, and the stability of the lithium ion battery is ensured.
The above-mentioned MnO based2Preferably, the high-molecular conductive polymer is prepared by carrying out polymerization reaction on 75-95% of polymerized monomers, 1-15% of PVA, 1-10% of deionized water, 2-10% of cross-linking agent and 0.1-5% of initiator; the polymeric monomer comprises one or more of acrylic acid, polyacrylic acid, methyl acrylate, isobutyl acrylate, and ethyl methacrylate.
The above-mentioned MnO based2-positive electrode sheet of lithium ion battery of PEDOT, preferably, GN is bound in the network structure of the binder of the high molecular polymer; the weight of GN is 1% -10% of the weight of the polymerized monomer. In the invention, the nano graphite is used as a conductive filler to prepare the anode slurry of the lithium ion battery. The addition of GN can greatly improve the conductivity of the high-purity polymerized monomer ionic liquid gel, and when the GN content is 6.0%, the resistivity of the composite material is about 3.025 omega cm, which is four orders of magnitude higher than that of polyacrylic gel.
The above-mentioned MnO based2-positive electrode sheet of lithium ion battery of PEDOT, preferably said cross-linking agent comprises dimethylsiloxane and one or more of dimethyldimethoxysilane, trimethyl borate and trimethyl phosphite.
The above-mentioned MnO based2-a positive plate of a lithium ion battery of PEDOT, preferably, the positive active material comprises a first positive active material and a second positive active material, the first positive active material is selected from one or more of lithium nickel cobalt manganese ternary material, lithium nickel cobalt aluminum ternary material and lithium-rich manganese-based material; the mass of the second positive electrode active material is 5% -50% of that of the first positive electrode active material; the second positive electrode active material particles are selected from one or more of lithium cobaltate, lithium nickel manganese oxide, lithium iron phosphate, lithium iron oxide and lithium manganese iron phosphate.
The above-mentioned MnO based2-positive plate of lithium ion battery of PEDOT, preferably, said electrical conductivityThe agent is selected from one or more of conductive carbon black, superconducting carbon black, conductive graphite, acetylene black, Ketjen black, graphene and carbon nano tubes.
The above-mentioned MnO based2-positive electrode sheet of lithium ion battery of PEDOT, preferably, the positive electrode slurry further comprises additives comprising cross-linked polydimethylsiloxane and one or more of dimethyldimethoxysilane, trimethyl borate and trimethyl phosphite.
A method for manufacturing a positive plate of a lithium ion battery based on MnO2-PEDOT comprises the following steps: 1) preparing a nanometer MnO2 film, namely preparing 5-15mmol/L Mn (CH3COO)2 aqueous solution; performing electrochemical deposition reaction on the positive plate by using a cyclic voltammetry method by taking the positive plate as a working electrode, wherein the cyclic potential is 0-1.3V, the scanning rate is 40-60mV/s, and the cycle number is 8-15; thirdly, cleaning the positive plate after the second step for 2-4 times in ethanol, then cleaning the positive plate in deionized water, and drying the positive plate;
2) preparing a MnO2-PEDOT film, namely placing the positive plate which is subjected to the step 1) in 10mmol/L EDOT monomer solution, and performing electrochemical deposition reaction on the positive plate by using the positive plate as a working electrode and adopting a cyclic voltammetry method, wherein the cyclic potential is 0-1.5V, the scanning rate is 40-60mV/s, and the cycle frequency is 8-15 times; secondly, cleaning the obtained composite electrode in ethanol for 2-4 times and then cleaning the electrode in deionized water; thirdly, drying, namely drying for 1-10 hours in vacuum at the temperature of 60 ℃;
3) preparing positive electrode slurry, namely mixing a polymerization monomer, GN, a cross-linking agent, a conductive agent and a positive electrode active material, uniformly dispersing by ultrasonic, and adding a thermal initiator or a photoinitiator;
4) carrying out polymerization reaction under the condition of microwave heating or UV light irradiation; the microwave heating temperature is 65-100 ℃, and the time is more than 30 min; the irradiation time of the UV light is 30-300 s;
5) and (3) uniformly coating the slurry obtained in the step (4) on the positive plate obtained in the step (2) to obtain the positive plate of the lithium ion battery based on MnO 2-PEDOT.
In the above method for manufacturing the positive plate of the lithium ion battery, preferably, the drying in the step 1) is vacuum drying at 45-80 ℃ for 20min-1 h.
In the above method for producing a positive electrode sheet for a lithium ion battery, the photoinitiator preferably includes 2-hydroxy-2-methyl-1-phenylpropanone, α -ketoglutaric acid, 1-hydroxycyclohexylphenylketone, 2-methyl-2- (4-morpholinyl) -1- [4- (methylthio) phenyl ] -1-propanone, 2,4, 6-trimethylbenzoyl-diphenylphosphine oxide, ethyl 2,4, 6-trimethylbenzoylphenylphosphonate, 2-dimethylamino-2-benzyl-1- [4- (4-morpholinyl) phenyl ] -1-butanone, 2-hydroxy-2-methyl-1- [4- (2-hydroxyethoxy) phenyl ] -1-propanone, and a mixture thereof, One or more of methyl benzoylformate; the thermal initiator comprises one or more of hydrogen peroxide, persulfate, and hydroperoxide.
Compared with the prior art, the invention has the advantages that: the MnO 2-PEDOT-based lithium ion battery has the advantages of high specific capacity of the positive plate, high conductivity and good cycling stability.
Drawings
Fig. 1(a) is an SEM micrograph of the positive electrode sheet in example 1.
Fig. 1(b) is an enlarged schematic view of fig. 1 (a).
FIG. 1(c) is an SEM microscopic characterization view of a positive electrode sheet in a comparative example
Fig. 1(d) is an enlarged schematic view of fig. 1 (c).
FIG. 2 is a graph of cyclic voltammetry of the positive electrode sheets of example 1 and comparative example 1 under 20 mV/s.
FIG. 3 is a graph showing cycle life at a large current density of 1A/g for example 1 and comparative example 1.
Detailed Description
In order to facilitate an understanding of the present invention, the present invention will be described more fully and in detail with reference to the preferred embodiments, but the scope of the present invention is not limited to the specific embodiments described below.
Unless otherwise defined, all terms of art used hereinafter have the same meaning as commonly understood by one of ordinary skill in the art. The terminology used herein is for the purpose of describing particular embodiments only and is not intended to limit the scope of the present invention.
Example 1
The preparation method of the positive plate of the lithium ion battery based on MnO2-PEDOT comprises the following steps of 1) preparing a nanometer MnO2 film, and preparing 10mmol/L Mn (CH3COO)2 aqueous solution; performing electrochemical deposition reaction on the positive plate by using a cyclic voltammetry method by taking the positive plate as a working electrode, wherein the cyclic potential is 0-1.3V, the scanning rate is 40-60mV/s, and the cycle number is 10 times; thirdly, cleaning the positive plate obtained in the second step for 4 times in ethanol, then cleaning the positive plate in deionized water, and drying the positive plate;
2) preparing a MnO2-PEDOT film, namely placing the positive plate which is subjected to the step 1) in 10mmol/L EDOT monomer solution, and performing electrochemical deposition reaction on the positive plate by using the positive plate as a working electrode and adopting a cyclic voltammetry method, wherein the cyclic potential is 0-1.5V, the scanning rate is 50mV/s, and the cycle number is 10 times; washing the obtained composite electrode in ethanol for 4 times, and then washing the electrode in deionized water; thirdly, drying, namely drying for 5 hours in vacuum at the temperature of 60 ℃;
3) preparing anode slurry, namely mixing polyacrylic acid, GN, dimethyl siloxane, dimethyl dimethoxy silane, acetylene black and an anode active material, performing ultrasonic dispersion uniformly, and adding hydrogen peroxide;
4) carrying out polymerization reaction under the microwave heating condition; the microwave heating temperature is 90 ℃, and the time is more than 30 min; 5) And (3) uniformly coating the slurry obtained in the step (4) on the positive plate obtained in the step (2) to obtain the positive plate of the lithium ion battery based on MnO 2-PEDOT.
Comparative example 1 to verify the superiority of this example, comparative examples were fabricated in which a PEDOT film was deposited on the positive electrode sheet by cyclic voltammetry and then MnO was deposited2The conditions of the film and deposition are the same, and other steps are also the same.
MnO as shown in FIG. 1(a) and FIG. 1(b)2The PEDOT composite film layer has a large number of micropores on the surface, which is beneficial to the electrolyte to permeate into the electrode, so that the electrode is fully contacted with the electrolyte, and the capacitance characteristic of the electrode can be fully exerted.
As shown in FIG. 1(c)Respectively, an SEM microscopic characteristic diagram of the positive electrode sheet in the comparative example, and fig. 1(d) is an enlarged schematic diagram of fig. 1 (c). MnO can be seen from the figure2The nano particles are attached to the PEDOT film to form PEDOT-MnO2A film. PEDOT-MnO2The film does not have a large number of micropores.
As shown in fig. 2, which is a cyclic voltammogram of the positive electrode sheets of example 1 and comparative example 1 under the condition of 20mV/s, it can be seen from the graph that the area surrounded by the cyclic voltammogram of the positive electrode sheet of example 1 is relatively large, which indicates that example 1 has relatively large specific capacity.
FIG. 3 is a graph showing cycle life at a large current density of 1A/g for example 1 and comparative example 1. It can be seen from the figure that the positive electrode sheets of comparative example 1 and example 1 exhibited distinct cycle characteristics. The positive electrode sheet of comparative example 1 exhibited linear decay, and after 4000 cycles, the capacity decayed from 183.8mAh/g to 82.4mAh/g, with a capacity decay rate of 55.16%. This is due to PEDOT-MnO2PEDOT layer and MnO in thin films2The layers are simply superposed on physical layers and do not form organic combination, and when the composite film is subjected to long-time cyclic charge and discharge, PEDOT is continuously stretched and extruded to generate irreversible microscopic deformation, so that the capacity is rapidly attenuated. And MnO2PEDOT films are monolithic MnO from PEDOT2The nano-sheets are completely wrapped and polymerized to form a large-area PEDOT layer. Hence MnO2The PEDOT film is not simply an interlayer composite, but is formed with PEDOT-MnO2PEDOT three-layer composite nano-structured composite material is covered with PEDOT material to form PEDOT and MnO2And (4) organically combining. MnO2The material is PEDOT material which plays a role of mechanical support and is attached to MnO when the PEDOT material is in charge and discharge2PEDOT on the surface of the nanosheet cannot deform irreversibly, the composite electrode has good cycle characteristics, the capacity of the composite electrode film is attenuated from 221.6mAh/g to 188.2mAh/g after 4000 times of high-current charging and discharging, and the capacity retention rate is 84.93%.
Claims (10)
1. Based on MnO2Lithium ion of PEDOTThe positive plate of battery, its characterized in that: comprises a positive plate and nano MnO formed on the positive plate by adopting an electrochemical method2Thin film in MnO2PEDOT film formed on the film and uniformly coated on MnO2Positive electrode paste on the film; the positive electrode slurry comprises a positive electrode active material, a gel-like adhesive and a conductive agent; the gel-like adhesive is a high-molecular conductive polymer formed by polymerizing monomers.
2. The MnO-based of claim 12-positive plate of a lithium ion battery of PEDOT, characterized in that: the high molecular conductive polymer is prepared by carrying out polymerization reaction on 75-95% of polymerized monomer, 1-15% of PVA, 1-10% of deionized water, 2-10% of cross-linking agent and 0.1-5% of initiator; the polymeric monomer comprises one or more of acrylic acid, polyacrylic acid, methyl acrylate, isobutyl acrylate, and ethyl methacrylate.
3. The MnO-based of claim 22-positive plate of a lithium ion battery of PEDOT, characterized in that: GN is bound in a network structure of the high molecular polymer binder; the weight of GN is 1% -10% of the weight of the polymerized monomer.
4. The MnO-based of claim 22-positive plate of a lithium ion battery of PEDOT, characterized in that: the cross-linking agent comprises dimethyl siloxane and one or more of dimethyl dimethoxy silane, trimethyl borate and trimethyl phosphite.
5. The MnO-based of claim 12-positive plate of a lithium ion battery of PEDOT, characterized in that: the positive active material comprises a first positive active material and a second positive active material, wherein the first positive active material is selected from one or more of lithium nickel cobalt manganese ternary materials, lithium nickel cobalt aluminum ternary materials and lithium-rich manganese-based materials; the mass of the second positive electrode active material is 5% -50% of that of the first positive electrode active material; the second positive electrode active material particlesThe second positive electrode active material particles are selected from one or more of lithium cobaltate, lithium nickel manganese oxide, lithium iron phosphate, lithium iron oxide and lithium iron manganese phosphate.
6. The MnO 2-PEDOT-based positive plate for a lithium ion battery as claimed in claim 1, wherein: the conductive agent is selected from one or more of conductive carbon black, superconducting carbon black, conductive graphite, acetylene black, Ketjen black, graphene and carbon nanotubes.
7. The MnO 2-PEDOT-based positive plate for a lithium ion battery as claimed in claim 1, wherein: the positive electrode slurry also comprises an additive, wherein the additive comprises crosslinked polydimethylsiloxane and one or more of dimethyl dimethoxysilane, trimethyl borate and trimethyl phosphite.
8. A method for manufacturing a positive plate of a lithium ion battery based on MnO2-PEDOT is characterized in that: the method comprises the following steps: 1) the preparation of a nano MnO2 film,
preparing 5-15mmol/L Mn (CH3COO)2 aqueous solution;
performing electrochemical deposition reaction on the positive plate by using a cyclic voltammetry method by taking the positive plate as a working electrode, wherein the cyclic potential is 0-1.3V, the scanning rate is 40-60mV/s, and the cycle number is 8-15;
will complete the step
Cleaning the positive plate in ethanol for 2-4 times, cleaning the positive plate in deionized water, and drying the positive plate;
2) preparation of MnO2-PEDOT film,
placing the positive plate after the step 1) in 10mmol/L EDOT monomer solution, and performing electrochemical deposition reaction on the positive plate by using the positive plate as a working electrode and adopting cyclic voltammetry, wherein the cyclic potential is 0-1.5V, the scanning rate is 40-60mV/s, and the cycle number is 8-15;
cleaning the obtained composite electrode in ethanol for 2-4 times, and then cleaning the composite electrode in deionized water;
drying, namely drying for 1-10h in vacuum at the temperature of 60 ℃;
3) the preparation of the positive electrode slurry is carried out,
mixing a polymerization monomer, GN, a cross-linking agent, a conductive agent and a positive active material, uniformly dispersing by ultrasonic, and adding a thermal initiator or a photoinitiator;
4) carrying out polymerization reaction under the condition of microwave heating or UV light irradiation; the microwave heating temperature is 65-100 ℃, and the time is more than 30 min; the irradiation time of the UV light is 30-300 s;
5) and (3) uniformly coating the slurry obtained in the step (4) on the positive plate obtained in the step (2) to obtain the positive plate of the lithium ion battery based on MnO 2-PEDOT.
9. The method for manufacturing a positive electrode sheet of a lithium ion battery according to claim 8, characterized in that: the drying in the step 1) is vacuum drying at the temperature of 45-80 ℃ for 20min-1 h.
10. The method for manufacturing a positive electrode sheet of a lithium ion battery according to claim 8, characterized in that: the photoinitiator comprises 2-hydroxy-2-methyl-1-phenyl acetone, alpha-ketoglutaric acid, 1-hydroxycyclohexyl phenyl ketone, 2-methyl-2- (4-morpholinyl) -1- [4- (methylthio) phenyl ] -1-acetone, 2,4, 6-trimethylbenzoyl-diphenyl phosphine oxide, 2,4, 6-trimethylbenzoyl phenyl ethyl phosphonate, 2-dimethylamino-2-benzyl-1- [4- (4-morpholinyl) phenyl ] -1-butanone, 2-hydroxy-2-methyl-1- [4- (2-hydroxyethoxy) phenyl ] -1-acetone, alpha-hydroxy-2-methyl-1-phenyl-ketone, alpha-ketoglutaric acid, alpha-hydroxy-cyclohexyl phenyl ketone, 2-methyl-2- (4-morpholinyl) -1-methyl ketone, alpha-methyl-1-, One or more of methyl benzoylformate; the thermal initiator comprises one or more of hydrogen peroxide, persulfate, and hydroperoxide.
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| CN113827770B (en) * | 2020-06-23 | 2022-08-09 | 中国科学院上海硅酸盐研究所 | Manganese dioxide-poly (3, 4-ethylenedioxythiophene) biological coating capable of promoting bone activity and preparation method and application thereof |
| CN114447307B (en) * | 2022-02-10 | 2024-03-15 | 湖北亿纬动力有限公司 | Composite positive electrode material, preparation method thereof and electrochemical energy storage device |
| CN114613966A (en) * | 2022-03-23 | 2022-06-10 | 广州市虎头电池集团股份有限公司 | Honeycomb negative electrode material and preparation method thereof |
| CN114695882A (en) * | 2022-05-02 | 2022-07-01 | 蔡梅 | Flexible lithium iron phosphate positive electrode material for bendable electronic equipment and preparation method |
| CN118016885A (en) * | 2024-02-01 | 2024-05-10 | 江西金糠新材料科技有限公司 | Positive electrode active material additive and preparation method and application thereof |
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