CN115000342A - Lithium-sulfur battery positive electrode with double capture function and preparation method and application thereof - Google Patents
Lithium-sulfur battery positive electrode with double capture function and preparation method and application thereof Download PDFInfo
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- CN115000342A CN115000342A CN202210519760.8A CN202210519760A CN115000342A CN 115000342 A CN115000342 A CN 115000342A CN 202210519760 A CN202210519760 A CN 202210519760A CN 115000342 A CN115000342 A CN 115000342A
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- 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
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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
- H01M10/00—Secondary cells; Manufacture thereof
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
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- 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
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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
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- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
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Abstract
The invention relates to a lithium-sulfur battery anode with a dual capture function, and a preparation method and application thereof. The positive electrode of the lithium-sulfur battery comprises an electrode active material, a current collector, a conductive agent and a binder with double capture functions of lithium polysulfide and polysulfide ion free radicals, wherein the binder is selected from one of polyaspartic acid-astaxanthin and polyaspartic acid-arbutin. The preparation method comprises the processing steps of dry powder mixing, slurry preparation, coating, drying and the like. The positive electrode of the lithium-sulfur battery has double capture functions of lithium polysulfide and polysulfide ion free radicals, can obviously inhibit the shuttle effect existing in the lithium-sulfur battery, and improves the charge-discharge efficiency, the discharge capacity and the cycle performance of the lithium-sulfur battery. In addition, the method has the advantages of compatibility with the existing lithium ion battery generation process, easily-controlled conditions, suitability for industrial production and the like.
Description
Technical Field
The invention relates to the technical field of lithium-sulfur batteries, in particular to a positive electrode with double capture functions of lithium polysulfide and polysulfide ion free radicals, and a preparation method and application thereof.
Background
With the increasing demand for energy storage in various technical applications such as portable electronic devices, electric vehicles, hybrid vehicles, and the like, research and development of high specific energy lithium batteries have been paid extensive attention by researchers. Among them, lithium-sulfur batteries are considered to be one of the most promising next-generation high-energy battery systems due to their high theoretical specific capacity (1675 mAh/g) and high energy density (2600 Wh/kg). The theoretical capacity of the active substance sulfur is that of the current commercial intercalation compound (LiCoO) 2 And LiFePO 4 ) And more than five times of the anode material. Meanwhile, the sulfur has rich reserves and low price, and the sulfur has the characteristic of environmental friendliness and has natural advantages when used as a battery material. However, lithium sulfur batteries also have certain problems: 1) the destruction of the electrode structure caused by the volume expansion of 80% in the electrode charging and discharging process; 2) the electronic and ionic conductivity of elemental sulfur is poor; 3) long-chain lithium polysulfide is easily dissolved in electrolyte, migrates between a positive electrode and a negative electrode and reacts with a lithium negative electrode, so that active substances are lost, and the performance of the battery is seriously attenuated. Among them, the dissolution of lithium polysulfide and the shuttle effect have drawn extensive attention from researchers due to the severity of their influence, and how to inhibit the shuttle effect has become a hotspot in the research field of lithium sulfur batteries. Achieving long cycle life, high energy density electrodes are critical.
However, in practical application of the lithium-sulfur battery, active sulfur of the positive electrode generates lithium polysulfide in a redox process, and the lithium polysulfide is dissolved in an electrolyte and dissociates into polysulfide ion radicals, so that loss is caused. In addition, lithium polysulfide and polysulfide ion free radicals can penetrate through the diaphragm and diffuse to the negative electrode, and after reaching the negative electrode, the lithium polysulfide and polysulfide ion free radicals generate side reaction with metal lithium to passivate the interface of the negative electrode, so that the electrochemical performance of the battery is further reduced. Therefore, how to inhibit the "shuttling effect" of lithium polysulfides and polysulfide ion radicals is crucial in lithium sulfur battery research.
The binder is used as an important component in the lithium-sulfur battery, and the mechanical property, viscoelasticity and structural characteristics of the binder have important influence on the electrochemical performance of the battery in the battery cycling process. The binder in the traditional electrode, such as polyvinylidene fluoride (PVDF), polyvinylpyrrolidone (PVP), sodium carboxymethylcellulose (CMC), Polytetrafluoroethylene (PTFE), polyethylene oxide (PEO), LA136, etc., has no binding and capturing effect on polysulfide ion free radicals, and thus cannot inhibit performance degradation of the lithium-sulfur battery due to the shuttle effect. Recently, Cuisinier and Zhang et al (adv. Energy Mater. 2015, 5, 1401801; ACS Energy Lett. 2021, 6, 537) reported the existence of polysulfide ion free radicals and their effect on the electrochemical performance of lithium-sulfur batteries, respectively, in the study of dissolution and shuttling of lithium polysulfides. Therefore, the lithium-sulfur battery electrode with the double capture functions of lithium polysulfide and polysulfide ion free radicals is designed, the shuttle effect of the lithium-sulfur battery is obviously inhibited, the capacity and the cycle performance of the lithium-sulfur battery are improved, and the lithium-sulfur battery electrode has important significance.
Disclosure of Invention
The invention aims to provide a positive electrode with double capture functions of lithium polysulfide and polysulfide ion free radicals, a preparation method and application thereof, and the capacity and the cycle performance of a lithium-sulfur battery are improved by inhibiting the shuttle effect existing in the lithium-sulfur battery.
In order to solve the above technical problems, according to one aspect of the present invention, there is provided a positive electrode for a lithium-sulfur battery having a dual trapping function, including an electrode active material, a current collector, a conductive agent, and a binder having a dual trapping function of lithium polysulfide and polysulfide ion radicals, the binder being selected from one of polyaspartic acid-astaxanthin and polyaspartic acid-arbutin.
Furthermore, the mass part ratio of the electrode active substance to the conductive agent to the binder is (8-9) to (0.05-1).
Further, the electrode active material is in the form of active sulfur or a sulfur/carbon composite.
Further, the current collector is an aluminum foil.
Further, the conductive agent is selected from one or a mixture of two of conductive carbon black and carbon nano tubes.
According to another aspect of the present invention, there is provided a method for preparing a positive electrode for a lithium-sulfur battery having a dual trapping function, comprising the steps of:
dispersing a binder into a solvent, stirring and preparing a uniformly mixed solution;
and step two, adding an electrode active substance and a conductive agent into the solution prepared in the step one, uniformly stirring to obtain positive electrode slurry, uniformly coating the positive electrode slurry on a current collector through a coating machine, and drying in vacuum to obtain the lithium-sulfur battery positive electrode.
Further, in the first step, the solvent is NMP (N-methylpyrrolidone) or DMF (N, N-dimethylformamide).
Further, in the second step, the vacuum drying temperature is 50-60 ℃.
According to another aspect of the present invention, there is provided a use of the above-described lithium sulfur battery positive electrode having a dual trapping function in the preparation of a lithium sulfur battery.
According to another aspect of the present invention, there is provided a lithium sulfur battery including the lithium sulfur battery positive electrode having the dual trapping function described above.
Compared with the prior art, the lithium-sulfur battery anode provided by the invention has the normal charge and discharge functions of a common sulfur lithium battery anode, and also has the double capture functions of lithium polysulfide and polysulfide ion free radicals, so that the shuttle effect existing in the lithium-sulfur battery can be obviously inhibited, and the charge and discharge efficiency, the discharge capacity and the cycle performance of the lithium-sulfur battery can be obviously improved. In addition, the method has the advantages of compatibility with the existing lithium ion battery generation process, easily-controlled conditions, suitability for industrial production and the like.
Drawings
FIG. 1 is a scanning electron micrograph of a positive electrode prepared using a polyaspartic acid-astaxanthin binder prepared in example 1;
FIG. 2 is a scanning electron micrograph of a positive electrode prepared using a polyaspartic acid-arbutin binder prepared in example 2;
fig. 3 is a scanning electron microscope image of a positive electrode prepared using a polyvinylidene fluoride binder, prepared in a comparative example;
fig. 4 is a graph of electrochemical impedance of assembled CR2032 button cells of examples 1, 2 and comparative example;
fig. 5 is a graph of the cycling performance of the CR2032 button cells of examples 1, 2 and pairs 1-3.
Detailed Description
An exemplary embodiment of the present invention provides a positive electrode for a lithium-sulfur battery having a dual trapping function, including an electrode active material, a current collector, a conductive agent, and a binder having a dual trapping function of lithium polysulfide and polysulfide ion radicals, the binder being selected from one of polyaspartic acid-astaxanthin and polyaspartic acid-arbutin.
Wherein the structural formula of the polyaspartic acid-astaxanthin is as follows:
wherein the structural formula of the polyaspartic acid-arbutin is as follows:
the active sites of the amino groups and the hydroxyl polar groups existing in the structural formulas of the polyaspartic acid-astaxanthin and the polyaspartic acid-arbutin in the binder have the function of capturing lithium polysulfide, and the benzoquinone-like structure has the function of capturing free radicals of polysulfide ions.
Wherein the mass part ratio of the electrode active substance to the conductive agent to the binder is (8-9) to (0.05-1), and the preferred mass part ratio of the electrode active substance to the conductive agent to the binder is (8-8.8): (0.2-1): 1, e.g., 8:1:1, 8:0.5:1, 8.8:0.2:1, 9:0.05: 0.05; further preferably, the mass part ratio of the electrode active material to the conductive agent to the binder is 8:1: 1.
Wherein, preferably, the electrode active material is in the form of active sulfur or a sulfur/carbon composite; the current collector is an aluminum foil; the conductive agent is selected from one or a mixture of two of conductive carbon black and carbon nano tubes.
The preparation method of the lithium-sulfur battery positive electrode with the double capture function comprises the following steps:
step one, dispersing the binder into a solvent, stirring and preparing into a uniformly mixed solution. The solvent is NMP (N-methylpyrrolidone) or DMF (N, N-dimethylformamide).
And step two, adding an electrode active substance and a conductive agent into the homogeneous solution prepared in the step one, uniformly stirring, uniformly coating the obtained positive electrode slurry on a current collector through a coating machine, and drying in vacuum to obtain the battery positive electrode. The vacuum drying temperature is 50-60 ℃. The coating thickness is preferably 100 to 250 μm.
The preparation method of the composite electrode active substance comprises the following steps: adding the electrode active substance and the host material into a planetary ball mill, mixing uniformly, and heating in a reaction kettle under inert atmosphere to obtain the composite material. For example: and (3) carrying out ball milling on the sublimed sulfur and the porous material, and keeping the sublimed sulfur and the porous material in a polytetrafluoroethylene reaction kettle for 48 hours at 150 ℃ under the atmosphere of argon to obtain the sulfur/carbon composite material.
The technical solution claimed by the present invention is further illustrated by the following examples. The examples are intended to illustrate embodiments of the invention without departing from the scope of the subject matter of the invention, and the scope of protection is not limited by the examples. Unless otherwise specifically indicated, the materials and reagents used in the present invention are available from commercial products in the art.
Example 1
(1) Ball-milling 5 g of sublimed sulfur and 2 g of porous carbon material in a ball mill at the rotating speed of 200 r/min for 4 h, keeping the mixture in a polytetrafluoroethylene reaction kettle at 150 ℃ for 48 h under the atmosphere of argon, and reserving the obtained sulfur/carbon composite material for later use.
(2) 0.1 g of polyaspartic acid-astaxanthin binder was added to 4 ml of NMP solvent and sufficiently dissolved by heating and stirring at 40 ℃ for use.
(3) And then adding 0.80 g of the prepared sulfur/carbon composite material and 0.1 g of carbon nano tube conductive agent into the solution, continuously heating and stirring for 30 hours, uniformly coating the slurry on an aluminum foil by using a coating knife with the thickness of 100 micrometers, drying for 48 hours in a vacuum drying oven at 50 ℃, and evaporating the solvent to obtain the lithium-sulfur battery pole piece with the double capturing functions of lithium polysulfide and polysulfide ion free radicals.
Example 2
(1) Ball-milling 5 g of sublimed sulfur and 2 g of porous carbon material in a ball mill at the rotating speed of 200 r/min for 4 h, and keeping the mixture in a polytetrafluoroethylene reaction kettle at 150 ℃ for 48 h under the atmosphere of argon to obtain the sulfur/carbon composite material.
(2) 0.10 g of polyaspartic acid-arbutin (URA-PASP) binder was added to 4 ml of DMF solvent and stirred at 40 ℃ to be sufficiently dissolved for use.
(3) And then adding 0.8 g of the prepared sulfur/carbon composite material and 0.1 g of acetylene black conductive agent into the solution, continuously stirring for 30 hours at room temperature, uniformly coating the slurry on an aluminum foil by using a coating knife with the thickness of 250 micrometers, drying for 72 hours in a vacuum drying oven at the temperature of 60 ℃, and evaporating the solvent to obtain the lithium-sulfur battery pole piece with the double capturing functions of lithium polysulfide and polysulfide ion free radicals.
Example 3
(1) Ball-milling 5 g of sublimed sulfur and 2 g of carbon black material in a ball mill at the rotating speed of 200 r/min for 4 h, and keeping the mixture in a polytetrafluoroethylene reaction kettle at 150 ℃ for 48 h under the atmosphere of argon to obtain the sulfur/carbon composite material.
(2) 0.10 g of polyaspartic acid-arbutin (URA-PASP) binder was added to 4 ml of N, N-dimethylformamide solvent and stirred at 40 ℃ to be sufficiently dissolved for use.
(3) And then adding 0.88 g of the prepared sulfur/carbon composite material and 0.02 g of the carbon nano tube conductive agent into the solution, continuously stirring for 30 hours at room temperature, uniformly coating the slurry on an aluminum foil by using a coating knife with the thickness of 200 mu m, drying for 72 hours in a vacuum drying oven at the temperature of 60 ℃, and evaporating the solvent to obtain the lithium-sulfur battery pole piece with the double capturing functions of lithium polysulfide and polysulfide ion free radicals.
Example 4
(1) Ball-milling 5 g of sublimed sulfur and 2 g of porous carbon material in a ball mill at the rotating speed of 200 r/min for 4 h, and keeping the mixture in a polytetrafluoroethylene reaction kettle at 150 ℃ for 48 h under the atmosphere of argon to obtain the sulfur/carbon composite material.
(2) 0.1 g of polyaspartic acid-astaxanthin binder was added to 4 ml of NMP (N-methylpyrrolidone) solvent and heated with stirring at 40 ℃ to be sufficiently dissolved for use.
(3) And then adding 1.0g of the prepared sulfur/carbon composite material and 0.1 g of carbon nano tube conductive agent into the solution, continuously heating and stirring for 30 hours, uniformly coating the slurry on an aluminum foil by using a coating knife with the thickness of 100 micrometers, drying for 48 hours in a vacuum drying oven at 50 ℃, and evaporating the solvent to obtain the lithium-sulfur battery pole piece with the double capturing functions of lithium polysulfide and polysulfide ion free radicals.
Comparative example
(1) And adding 5 g of sublimed sulfur and 2 g of activated carbon material into a mixer, fully grinding for 2 h, and uniformly mixing to obtain the sulfur/carbon composite material for later use.
(2) 0.1 g of polyvinylidene fluoride binder was added to 4 ml of N-methylpyrrolidone solvent and stirred at room temperature to be sufficiently dissolved for use.
(3) And then adding 0.8 g of the prepared sulfur/carbon composite material into the solution, continuously stirring at room temperature for 24 hours, uniformly coating the slurry on an aluminum foil by using a coating knife with the thickness of 250 micrometers, drying in a vacuum drying oven at the temperature of 60 ℃ for 48 hours, and evaporating the solvent to obtain the lithium-sulfur battery pole piece prepared by adopting the traditional binder.
And assembling the prepared pole piece in the embodiment into a CR2032 type button cell to perform corresponding cell performance test. The battery structure comprises a cathode shell, an anode plate, electrolyte, a diaphragm, electrolyte, a lithium plate, a gasket, a spring piece and an anode shell which are assembled in sequence. Wherein the positive electrode is S @ CNT composite material, the negative electrode is lithium sheet, the electrolyte is (1 mol/L LiTFSI, volume ratio V (DOL): V (DME) = 1:1, and the like1% LiNO was added 3 ）。
It can be observed from fig. 1-3 that the positive electrode surface prepared by using the polyaspartic acid-astaxanthin binder forms many "bridges" between the electrode active material and the conductive agent, which indicates that the binder plays a good role in connection, and the electrode surface is more dense. 2-3, it can be observed that the surface of the positive electrode has many holes and cracks, which will cause the problems of positive electrode collapse, rapid capacity decay, short service life, etc. during the cycling process of the battery; by comparing the three components in FIG. 4, it can be found that the charge transfer resistance of the polyaspartic acid-astaxanthin system is the minimum, which is more beneficial to the transmission of lithium ions in the battery; from FIG. 5, it can be seen that the initial capacity of the polyaspartic acid-astaxanthin system battery can reach 1390 mAh g -1 About, the capacity can be stabilized at 1200 mAh g after 25 circles of circulation -1 On the other hand, the initial capacity of the PVDF battery is only 750 mAh g -1 The capacity of the two is very different. In conclusion, the polyaspartic acid-astaxanthin binding agent with the double capture functions of lithium polysulfide and polysulfide ion free radicals has better effect.
Claims (10)
1. A lithium-sulfur battery positive electrode having a dual trapping function, characterized in that: the electrode comprises an electrode active material, a current collector, a conductive agent and a binder with double capture functions of lithium polysulfide and polysulfide ion free radicals, wherein the binder is selected from one of polyaspartic acid-astaxanthin and polyaspartic acid-arbutin.
2. The positive electrode for a lithium sulfur battery having a dual trapping function according to claim 1, characterized in that: the mass part ratio of the electrode active substance to the conductive agent to the binder is (8-9) to (0.05-1).
3. The positive electrode for a lithium sulfur battery having a dual trapping function according to claim 1, characterized in that: the electrode active material is active sulfur or a sulfur/carbon composite material.
4. The positive electrode for a lithium sulfur battery having a dual trapping function according to claim 1, characterized in that: the current collector is aluminum foil.
5. The positive electrode for a lithium sulfur battery having a dual trapping function according to claim 1, characterized in that: the conductive agent is selected from one or a mixture of two of conductive carbon black and carbon nano tubes.
6. The method for preparing a positive electrode for a lithium-sulfur battery having a dual trapping function according to claims 1 to 5, comprising the steps of:
dispersing a binder into a solvent, stirring and preparing a uniformly mixed solution;
and step two, adding an electrode active substance and a conductive agent into the solution prepared in the step two, uniformly stirring to obtain positive electrode slurry, uniformly coating the positive electrode slurry on a current collector through a coating machine, and drying in vacuum to obtain the lithium-sulfur battery positive electrode.
7. The method of claim 6, wherein: and in the second step, the solvent is NMP (N-methylpyrrolidone) or DMF (N, N-dimethylformamide).
8. The method of claim 6, wherein: in the third step, the vacuum drying temperature is 50-60 ℃.
9. Use of the lithium sulfur battery positive electrode with dual capture function according to any one of claims 1 to 5 for the preparation of a lithium sulfur battery.
10. A lithium sulfur battery, characterized by: a lithium-sulfur battery positive electrode having a dual trapping function comprising any one of claims 1 to 5.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN108155383A (en) * | 2017-11-29 | 2018-06-12 | 中山大学 | A kind of lithium-sulfur cell binding agent and preparation method thereof and lithium-sulphur cell positive electrode |
| US20180175366A1 (en) * | 2015-06-26 | 2018-06-21 | Florida State University Research Foundation, Inc. | Dry process method for producing electrodes for electrochemical devices and electrodes for electrochemical devices |
| CN109768280A (en) * | 2018-12-20 | 2019-05-17 | 中国科学院青岛生物能源与过程研究所 | A kind of lithium battery anode with free radical capture function |
| CN113178560A (en) * | 2021-05-11 | 2021-07-27 | 湖北亿纬动力有限公司 | Metal oxide coated NCM ternary electrode material, preparation method thereof and lithium ion battery |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20180175366A1 (en) * | 2015-06-26 | 2018-06-21 | Florida State University Research Foundation, Inc. | Dry process method for producing electrodes for electrochemical devices and electrodes for electrochemical devices |
| CN108155383A (en) * | 2017-11-29 | 2018-06-12 | 中山大学 | A kind of lithium-sulfur cell binding agent and preparation method thereof and lithium-sulphur cell positive electrode |
| CN109768280A (en) * | 2018-12-20 | 2019-05-17 | 中国科学院青岛生物能源与过程研究所 | A kind of lithium battery anode with free radical capture function |
| CN113178560A (en) * | 2021-05-11 | 2021-07-27 | 湖北亿纬动力有限公司 | Metal oxide coated NCM ternary electrode material, preparation method thereof and lithium ion battery |
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