CN115832617A - Intercalation composite film, preparation method thereof and lithium-sulfur battery - Google Patents
Intercalation composite film, preparation method thereof and lithium-sulfur battery Download PDFInfo
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Abstract
The invention discloses an intercalation composite film, a preparation method thereof and a lithium-sulfur battery. The intercalation composite film can be applied to a lithium-sulfur battery, can be particularly clamped between a positive plate and a diaphragm of the lithium-sulfur battery, can adsorb polysulfide dissolved in electrolyte in the battery charging process, inhibits the shuttle effect of the lithium-sulfur battery, can provide good conductivity when the conductive base layer is used as a support body, can utilize the adsorbed polysulfide, and improves the utilization rate of active substances, thereby improving the performance of the lithium-sulfur battery.
Description
Technical Field
The invention relates to the technical field of batteries, in particular to an intercalation composite film, a preparation method thereof and a lithium-sulfur battery.
Background
The lithium-sulfur battery has extremely high theoretical specific capacity (1675 mAh/g) and theoretical energy density (2600 Wh kg) -1 ) And it is cheap and environmentally friendly, thus has received extensive attention and research from the scientific and industrial circles. The lithium-sulfur battery is a secondary battery system with a lithium simple substance as a negative electrode and a sulfur simple substance or sulfur-based composite material as a positive electrode. During the discharge process of the battery, the positive electrode sulfur-based material can form a plurality of chain polysulfides in the process of redox reaction, the polysulfides can be dissolved in the electrolyte, can diffuse and migrate to the negative electrode side through the diaphragm by taking the electrolyte as a medium due to concentration difference, and can be reduced into insulating and insoluble Li 2 S 2 And Li 2 S is then coated on the surface of the negative electrode, thereby causing a "shuttle effect". This material does not allow the system to draw current, and therefore, the utilization rate of the active materials, namely, the negative electrode lithium and the positive electrode sulfur, is reduced, and the battery performance is affected. In this regard, there is a strong need to find a solution to the above problems.
Disclosure of Invention
The present invention is directed to solving at least one of the problems of the prior art. Therefore, the invention provides an intercalation composite film, a preparation method thereof and a lithium-sulfur battery.
In a first aspect of the present invention, an intercalation composite film is provided, which comprises a conductive base layer, wherein zinc oxide is loaded inside and on the surface of the conductive base layer.
The intercalation composite film according to the embodiment of the invention has at least the following beneficial effects: the intercalation composite film comprises a conductive base layer and zinc oxide loaded in and on the conductive base layer, can be applied to a lithium-sulfur battery, and can be particularly clamped between a positive plate and a diaphragm of the lithium-sulfur battery, and in the charging process of the battery, the zinc oxide can adsorb polysulfide dissolved in electrolyte, so that the phenomenon that the dissolved polysulfide diffuses and migrates to the negative pole side to generate side reaction to generate insulating and insoluble Li is reduced or even avoided 2 S 2 And Li 2 The S is covered on the surface of the negative electrode, so that the shuttle effect of the lithium-sulfur battery is inhibited; and the conductive base layer can be used as a support body, can provide good conductivity, and can utilize the adsorbed polysulfide to improve the utilization rate of active substances, so that the performance of the lithium-sulfur battery is improved, including the improvement of electrochemical reversibility, multiplying power cycle performance and cycle stability, and the reduction of capacity attenuation.
The conductive base layer has a pore structure, wherein the pore can be an interlayer pore of the conductive base layer with a laminated structure or an internal pore of the conductive base layer with a pore structure; the zinc oxide is specifically supported in the internal pores and on the surface of the conductive base layer. In some embodiments of the invention, the electrically conductive substrate is selected from at least one of graphite paper, carbon fiber paper, carbon cloth. Preferably, the conductive substrate is selected from graphite paper, which has a layered structure, and zinc oxide is supported between layers (i.e., between graphite sheets) and on the surface of the graphite paper.
In some embodiments of the invention, the zinc oxide is nano zinc oxide. Preferably, the nano zinc oxide is a flower cluster-shaped zinc oxide nano material, and the nano zinc oxide in the form has a larger specific surface area, so that the adsorption efficiency of polysulfide can be improved. For the conductive base layer graphite paper with a laminated structure, zinc oxide layers can be formed between graphite sheet layers and on the surface of the graphite sheet layers of the nano zinc oxide loaded graphite paper, and the thickness of the zinc oxide layers can be controlled to be 200-500 nm.
In some embodiments of the invention, the thickness of the intercalated composite film is 15 to 30 μm; typically about 20 μm or so.
In a second aspect of the present invention, a method for preparing any one of the intercalated composite thin films provided in the first aspect of the present invention is provided, comprising the following steps:
s1, taking a conductive base layer as a working electrode, and matching the conductive base layer and a first counter electrode in a first electrolyte for electrolysis;
s2, electrochemically depositing metal zinc in the conductive base layer obtained by the step S1 and on the surface of the conductive base layer;
and S3, calcining the membrane material obtained in the step S2 to convert the metal zinc into zinc oxide, and preparing the intercalation composite film.
The preparation method of the intercalation composite film according to the embodiment of the invention has at least the following beneficial effects: the preparation method comprises the steps of electrolyzing the conductive base layer to open the structure of the conductive base layer (if the conductive base layer is a conductive base layer with a layered structure, a sheet layer of the conductive base layer can be opened through electrolysis), so that more sites are provided for the adhesion of zinc oxide, and the uniform deposition of zinc ions is facilitated; then, metal zinc is uniformly deposited in and on the surface of the electrolyzed conductive base layer through electrochemical deposition, and then the metal zinc is converted into zinc oxide through calcination, so that the uniform and stable loading of the zinc oxide on and in the conductive base layer is realized, and the obtained zinc oxide is in a regularly-arranged flower cluster-shaped structure and has a large specific surface area; the process is simple, convenient for production operation and suitable for large-scale production; by the method, the obtained product intercalation composite film can keep the complete structure of the conductive base layer (such as the complete layered structure of graphite paper) so as to enable the film to have an independent self-supporting structure; the intercalation composite film can be applied to a lithium-sulfur battery, and particularly can be clamped between a positive plate and a diaphragm, and zinc oxide on the intercalation composite film can effectively adsorb dissolved polysulfide in the discharging process of the battery, so that the shuttle effect of the lithium-sulfur battery is inhibited; and the conductive base layer can provide good conductivity while serving as a support body, so that the adsorbed polysulfide is utilized, the utilization rate of active substances is improved, and the performance of the lithium-sulfur battery is improved.
In some embodiments of the present invention, in step S1, the first electrolyte is at least one selected from a sulfuric acid solution, a hydrochloric acid solution, and a nitric acid solution. The thickness of the conductive base layer can be controlled to be 10-20 μm, generally about 18 μm; the first pair of electrodes may employ platinum electrodes. After electrolysis, further cleaning treatment can be carried out, and specifically, deionized water can be adopted to rinse the conductive base layer.
In some embodiments of the present invention, in step S2, the zinc salt solution is used as the second electrolyte, the conductive base layer is used as the second working electrode, and the conductive base layer is used in cooperation with the second counter electrode for electrochemical deposition. The nano-scale material can be prepared by electrochemical deposition, and the method is simple to operate, low in cost and high in efficiency; and the uniform load of the metal zinc can be realized, and the complete and smooth surface of the conductive base layer can be kept. Wherein, the second pair of electrodes can adopt platinum electrodes. Specifically, the nano zinc oxide layer with the thickness of about 200-500 nm can be prepared through electrochemical deposition, and if graphite paper is used as a conductive base layer, the thickness can be increased by 2-4 μm after electrolysis and electrochemical deposition in the steps S1 and S2.
In some embodiments of the invention, the zinc salt solution is selected from at least one of zinc sulfate solution, zinc chloride solution, zinc nitrate solution.
In some embodiments of the invention, the calcining is firing the film material in air using an alcohol lance.
In a third aspect of the invention, a lithium sulfur battery is provided, which comprises a positive plate, a diaphragm and a negative plate which are sequentially stacked; the lithium ion battery also comprises an intercalation composite film prepared by any one of the intercalation composite films or the preparation method of any one of the intercalation composite films, and the intercalation composite film is arranged between the positive plate and the diaphragm.
The positive plate can comprise a positive current collector and a positive active material layer coated on the surface of the positive current collector, the positive active material layer can comprise a sulfur-based positive active material, a conductive agent and a binder, and the sulfur-based positive active material can be sulfur elementary substance or sulfur-based composite material. Sulfur as a positive electrode active material has low conductivity, which leads to a decrease in the utilization rate of sulfur as an active material and a decrease in the cycle performance of a battery, and the use efficiency of the active material can be improved by sufficiently contacting the active material with the addition of a conductive agent. The conductive agent may specifically be conductive carbon black, carbon nanotubes, or the like. In addition, the addition of the binder can better combine the active material with the conductive agent, enhance the conductivity and maintain the internal structure to be stable during the charge and discharge of the battery.
The diaphragm can be one or more composite films of polyethylene, polypropylene and polyvinylidene fluoride, but is not limited to the composite films and can also be other diaphragms.
Drawings
The invention is further described with reference to the following figures and examples, in which:
FIG. 1 is a schematic view of a flow chart for preparing an interlayer composite film in example 1;
FIG. 2 is a schematic view of an assembled structure of a lithium sulfur battery in example 2;
FIG. 3 is a surface SEM photograph of an intercalated composite film prepared in example 1;
FIG. 4 is a graph showing the results of the contact angle test between the graphite paper processed in step S1 of example 1 and the intercalated composite film finally obtained and the electrolyte;
FIG. 5 is a graph showing the test results of the intercalation composite film prepared in example 1 adsorbing polysulfide;
FIG. 6 is a graph showing the results of a test of the charge-discharge cycle performance of the lithium sulfur batteries of example 2 and comparative examples 1 and 2;
fig. 7 is a graph showing the results of different rate cycle performance tests of the lithium sulfur batteries of example 2 and comparative example 1.
Detailed Description
The concept and technical effects of the present invention will be clearly and completely described below in conjunction with the embodiments to fully understand the objects, features and effects of the present invention. It is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments, and other embodiments obtained by those skilled in the art without inventive efforts are within the protection scope of the present invention based on the embodiments of the present invention.
Example 1
In this embodiment, an intercalation composite film is prepared, as shown in fig. 1, and the preparation method specifically includes:
s1, preparing 0.1mol/L H 2 SO 4 The solution was then extracted 30mL of this H 2 SO 4 Putting the solution into a 50mL electrolytic tank A as electrolyte; one end of the electrode clamps graphite paper with the size of 1cm multiplied by 2cm and is used as a working electrode, and the other end of the electrode uses a platinum electrode with the same area as a counter electrode; immersing the graphite paper serving as a working electrode and the platinum electrode serving as a counter electrode in the electrolyte in the electrolytic tank A, and applying 5V direct current to electrolyze for 40s respectively on the front side and the back side of the graphite paper; then, the electrolyzed graphite paper is washed by deionized water for three times and is soaked in the deionized water for storage for later use;
s2, preparing ZnSO with 0.1mol/L 4 The solution was then extracted 30mL of the ZnSO 4 Putting the solution into a 50mL electrolytic tank B as electrolyte; clamping the graphite paper obtained in the step S1 by using an electrode at one end as a working electrode, and using platinum electrodes with the same area size as a counter electrode at the other end; immersing the graphite paper of the working electrode and the platinum electrode of the counter electrode in the electrolyte in the electrolytic tank B, applying 5V direct current to carry out electrochemical deposition, and depositing the front side and the back side of the graphite paper for 1min respectively; depositing on graphite paper to obtain regularly arranged flower cluster-shaped metallic zinc simple substances, repeatedly washing with deionized water for three times, and soaking in deionized water for 10min to remove redundant foreign ions such as free zinc ions and sulfate ions.
And S3, placing the graphite paper deposited with the metal zinc simple substance in the step S2 into a crucible, and burning the graphite paper in the air for 30S by using an alcohol spray gun to convert the metal zinc simple substance into zinc oxide so as to obtain the intercalation composite film.
Example 2
In this example, a lithium-sulfur battery is prepared, and the preparation method specifically includes:
s1, preparing a positive plate, which comprises the following steps:
(1) Weighing 150mg of battery-grade polyvinylidene fluoride (PVDF) powder, adding the powder into a small bottle, adding 9.5mL of N-methyl-2-pyrrolidone (NMP) serving as a solvent into a 10mL injector, adding a stirrer, stirring at room temperature for 4 hours to fully dissolve the powder, and placing the powder aside for later use;
(2) Respectively weighing 700mg of elemental sulfur of the positive electrode material and 200mg of conductive agent Super-P, then sucking 7mL of PVDF solution taking NMP as a solvent from a small bottle by using a syringe, adding the PVDF solution into a ball milling tank together, ball milling for 3 hours at a ball-material ratio of 50 at a rotating speed of 1032r/min, then collecting the ball-milled positive electrode slurry, and sealing;
(3) Dripping 0.5mL of alcohol on a 20X 20cm glass plate, placing an aluminum foil on the glass plate, then dripping about 0.5mL of alcohol on the aluminum foil, and wiping the aluminum foil with paper until the aluminum foil is flat; uniformly coating the above-prepared positive electrode slurry of about 2mL on an aluminum foil by using a scraper of 150 mm; drying for 12 hours at a 60 ℃ hot bench, and then performing roller pressing by using a roller press according to a compression ratio of 1: tabletting according to the proportion of 1.5; slicing the obtained positive plate with a slicer with 12mm diameter, weighing, and selecting active substances with mass of 1.1-1.2mg/cm 2 The left and right anode wafers are used as anode wafers and collected and placed in an argon glove box for later use. Wherein, the active substance mass is obtained by the following method: weighing and recording the cut positive plate to obtain a mass m1, cutting copper foils with the same area size to obtain a weight m2, wherein the mass of the active substance is equal to (m 1-m 2) × the active substance ratio;
s2, taking a lithium sheet as a negative electrode sheet, adopting a PP diaphragm as the diaphragm, and adopting an electrolyte containing 1M lithium bistrifluoromethanesulfonimide (LiTFSI) and 0.2M lithium nitrate (LiNO) 3 ) Specifically, as shown in fig. 2, a lithium sheet 12 is put into a positive electrode shell 11, a proper amount of electrolyte is added, a diaphragm 13 and an intercalation composite film 14 are sequentially put into the positive electrode shell, then the electrolyte is dripped, a positive electrode sheet 15, a gasket 16 and an elastic sheet 17 are placed, and then a negative electrode shell 18 is used for pressing and assembling to obtain the button cell, namely the product lithium-sulfur cell.
Comparative example 1
This comparative example, which differs from example 2 in that a lithium sulfur battery was prepared: this comparative example cancels the provision of the intercalation composite film between the separator and the positive electrode sheet in step S2, and the other operations are the same as in example 2.
Comparative example 2
This comparative example, which differs from example 2 in that a lithium sulfur battery was prepared: in the comparative example, in the step S2, the arrangement of the intercalation composite film between the diaphragm and the positive plate is cancelled; the surface of one side of the PP diaphragm is provided with a graphite zinc oxide coating, the PP diaphragm provided with the graphite zinc oxide coating is used as the diaphragm, and the side, provided with the graphite zinc oxide coating, of the diaphragm faces to the positive plate in the battery assembling process; the other operations were the same as in example 2.
The above separator in this comparative example was prepared by the method comprising: mixing graphite paper and zinc oxide, grinding the mixture in a mortar, and mixing the ground mixture with a binder and a solvent to prepare slurry, wherein the mass ratio of the binder to the graphite paper to the zinc oxide is 1:8:1, coating the surface of a PP diaphragm to a thickness of about 20 mu m, and drying to form a graphite tin oxide coating on the surface of the PP diaphragm.
Performance test
The surface of the intercalated composite film obtained in example 1 was observed by a Scanning Electron Microscope (SEM), and the result is shown in FIG. 3. As shown in fig. 3, the zinc oxide layer on the surface of the intercalated composite film prepared by the preparation method of example 1 has a flower-like structure arranged in order.
Taking the graphite paper obtained by the step S1 in the example 1 and the intercalation composite film finally prepared, respectively dropping a drop of lithium-sulfur electrolyte on the surfaces of the graphite paper and the intercalation composite film, and then testing the contact angles of the electrolyte, the electrolyzed graphite paper and the intercalation composite film, wherein the obtained result is shown in fig. 4. In fig. 4, (a) is the test result of the contact angle of the electrolyte and the graphite paper after electrolysis, and the contact angle is 34.6 degrees; (B) The contact angle of the electrolyte and the intercalation composite film is 23.1 degrees, so that the contact angle between the electrolyte and the intercalation composite film is smaller than that between the electrolyte and the electrolyzed graphite paper, and lithium ions can penetrate through the intercalation composite film more quickly, thereby being more beneficial to the electrochemical reaction.
In order to examine the adsorption performance of the intercalated composite film prepared in the present application to polysulfides, the intercalated composite film prepared in example 1 was placed in a yellowish polysulfide solution (prepared by reacting elemental sulfur and lithium sulfide in a molar ratio of 1. FIG. 5 (a) is a sample before adding an intercalated composite film to a polysulfide solution; (b) The sample is obtained after adding the intercalation composite film into polysulfide solution and standing for 1 h. The test results show that the color of the polysulfide solution changes from the original light yellow to clear and transparent after the intercalation composite film is added, because the zinc oxide in the intercalation composite film adsorbs the polysulfide dissolved in the electrolyte.
In addition, the charge and discharge cycle performance of the lithium sulfur batteries manufactured in example 2 and comparative examples 1 to 2 was tested at 0.2C rate with the voltage window set to 0 to 2.8V, and the results are shown in fig. 6. As can be seen from fig. 6, after 350 weeks of charge-discharge cycle at 0.2C rate, the lithium-sulfur battery of comparative example 1 has a capacity of 762.0mAh/g only without an intercalation composite film between the PP separator and the positive electrode sheet; example 2 the intercalation composite film of example 1 is sandwiched between the PP separator and the positive plate of the lithium-sulfur battery, the capacity of the battery after 350 weeks of charge-discharge cycle under 0.2C rate is still 1100.2mAh/g, and the capacity attenuation is significantly reduced; comparative example 2 a lithium-sulphur cell provided with a graphite zinc oxide coating on the side of the PP separator facing the positive plate had a capacity of 877.0mAh/g after 350 cycles of charge and discharge at 0.2C rate, which was higher than comparative example 1 but still significantly lower than example 2. From the above, in the lithium sulfur battery of embodiment 2, the intercalation composite film of embodiment 1 is sandwiched between the PP separator and the positive plate, wherein the zinc oxide is loaded between the layers and the surface of the graphite paper, the zinc oxide can adsorb the polysulfide generated by the sulfur-based positive active material in the redox process and dissolve the electrolyte, and the adsorbed polysulfide can be utilized through the good conductivity of the graphite paper, so that the utilization rate of the active material can be improved, the cycle performance of the battery can be improved, and the capacity attenuation can be reduced.
In addition, the rate cycle performance of the lithium sulfur batteries of example 2 and comparative example 1 was tested at current densities of 0.2C, 0.5C, 1C, 1.5C, and 2C, respectively, and the results are shown in fig. 7. As shown in fig. 7, the initial specific discharge capacity of the lithium-sulfur battery of comparative example 1 at a current density of 0.2C was 1110.6mAh/g, and the capacity was significantly decreased after 5 cycles; when the current density was increased to 0.5C, 1.0C, 1.5C and 2.0C, the discharge capacity was 864.3mAh/g, 647.7mAh/g, 519.2mAh/g and 438.9mAh/g, respectively. And the reversible specific capacities of the lithium-sulfur battery of the example 2 at the multiplying powers of 0.2C, 0.5C, 1C, 1.5C and 2C are 1238.1mAh/g, 1027.9mAh/g, 914.6mAh/g, 836.9mAh/g and 745.1mAh/g respectively. The comparison shows that the lithium-sulfur battery in the comparative example 1 is not provided with the intercalation composite film between the PP diaphragm and the positive plate, the rate performance of the battery is obviously inferior to that of the lithium-sulfur battery in the example 2, which can show that the electrode electrochemical reaction dynamic process is slower under higher current density, and lithium polysulfide shuttles to cause serious active substance loss in the test process, so that the reversible specific capacity of the battery is low under higher current density.
The above-mentioned embodiments only express several embodiments of the present invention, and the description thereof is more specific and detailed, but not construed as limiting the scope of the present invention. It should be noted that, for a person skilled in the art, several variations and modifications can be made without departing from the inventive concept, which falls within the scope of the present invention.
Claims (10)
1. The intercalated composite film is characterized by comprising a conductive base layer, wherein zinc oxide is loaded in the conductive base layer and on the surface of the conductive base layer.
2. The intercalated composite film as claimed in claim 1, wherein the conductive substrate layer is selected from at least one of graphite paper, carbon fiber paper and carbon cloth.
3. The intercalated composite film of claim 1 wherein said zinc oxide is nano zinc oxide.
4. The intercalated composite film as claimed in any one of claims 1 to 3 wherein the thickness of the intercalated composite film is 15 to 30 μm.
5. The process for preparing an intercalated composite film according to any one of claims 1 to 4, comprising the steps of:
s1, taking a conductive base layer as a working electrode, and matching the conductive base layer and a first counter electrode in a first electrolyte for electrolysis;
s2, electrochemically depositing metal zinc in the conductive base layer obtained by the step S1 and on the surface of the conductive base layer;
and S3, calcining the membrane material obtained by the treatment in the step S2 to convert the metal zinc into zinc oxide, thereby preparing the intercalation composite membrane.
6. The method of claim 5, wherein in step S1, the first electrolyte is at least one selected from a sulfuric acid solution, a hydrochloric acid solution, and a nitric acid solution.
7. The method for preparing an intercalated composite film according to claim 5, wherein in step S2, a zinc salt solution is used as a second electrolyte, the conductive base layer is used as a second working electrode, and the conductive base layer is matched with a second counter electrode for electrochemical deposition.
8. The method for preparing the intercalated composite film according to claim 7, wherein the zinc salt solution is at least one selected from the group consisting of zinc sulfate solution, zinc chloride solution and zinc nitrate solution.
9. The method of claim 5, wherein in step S3, the calcining is performed by burning the film material in air with an alcohol spray gun.
10. A lithium-sulfur battery comprising a positive electrode sheet, a separator and a negative electrode sheet, which are stacked, characterized by further comprising the intercalation composite film according to any one of claims 1 to 4 or the intercalation composite film produced by the method according to any one of claims 5 to 9, the intercalation composite film being sandwiched between the positive electrode sheet and the separator.
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| CN116936777A (en) * | 2023-09-15 | 2023-10-24 | 山东海化集团有限公司 | Positive and negative electrode materials of lithium-sulfur battery, and preparation method and application thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN116936777A (en) * | 2023-09-15 | 2023-10-24 | 山东海化集团有限公司 | Positive and negative electrode materials of lithium-sulfur battery, and preparation method and application thereof |
| CN116936777B (en) * | 2023-09-15 | 2023-12-29 | 山东海化集团有限公司 | Positive and negative electrode materials of lithium-sulfur battery, and preparation method and application thereof |
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