CN111416099B - Preparation method of soft-hard double-layer sulfur lithium battery anode - Google Patents
Preparation method of soft-hard double-layer sulfur lithium battery anode Download PDFInfo
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- CN111416099B CN111416099B CN202010237710.1A CN202010237710A CN111416099B CN 111416099 B CN111416099 B CN 111416099B CN 202010237710 A CN202010237710 A CN 202010237710A CN 111416099 B CN111416099 B CN 111416099B
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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
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/052—Li-accumulators
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- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
Abstract
The invention discloses a preparation method of a soft and hard double-layer lithium sulfur battery anode, which comprises the steps of firstly preparing porous carbon powder from egg white, stirring the prepared porous carbon powder into slurry by using a polytetrafluoroethylene binder, then coating the slurry on one side of a porous polypropylene film, and adhering a coating layer of the polypropylene film with the slurry to an original solid lithium sulfur battery anode to prepare a two-layer lithium sulfur battery anode, wherein the original lithium sulfur battery anode is solid, and the coated film anode is plastic, so that the soft and hard combined double-layer lithium sulfur battery anode is realized. The invention solves the problems of low efficiency and short service life of the battery in the prior art.
Description
Technical Field
The invention belongs to the technical field of batteries, and particularly relates to a preparation method of a soft and hard double-layer sulfur lithium battery anode.
Background
The sulfur lithium battery has large capacity and is environment-friendly, and is a potential commercial battery. Sulfur lithium batteries use sulfur as the anode, and because sulfur is not conductive, it is difficult to transport the lost electrons out, so composite electrodes have been used. The composite electrode is mostly a carbon and sulfur composite material, so that sulfur transfers lost electrons to the carbon material, the carbon material transfers the electrons out, but solid sulfur loses electrons and becomes a liquid sulfide, for example, S-S loses electrons and becomes liquid Li 2 S 8 ,Li 2 S 8 Continue to lose electrons to liquid Li 2 S 6 And in addition, the liquid sulfide can easily flow into the cathode of the battery, so that the sulfide which does not react completely can not continuously discharge, and the current efficiency of the sulfur lithium battery is greatly reduced. For the further research, the anode of the sulfur lithium battery is prepared into a porous structureAnd a material for keeping the generated liquid sulfide inside the small hole. The method well improves the efficiency of the sulfur lithium battery, but has the new problems that the volume of sulfide generated by sulfur reaction is increased by more than 2 times, the pores of the porous carbon-sulfur battery are collapsed due to volume expansion, the anode surface of the battery is reduced, the discharging speed is reduced, in addition, the volume expansion extrudes part of sulfide generated by reaction out of the pores, and the extruded sulfide partially flows to the cathode, so the shuttle effect is technically called, the efficiency of the battery is reduced, and the service life of the battery is shortened.
Disclosure of Invention
The invention aims to provide a preparation method of a soft-hard double-layer sulfur lithium battery anode, which solves the problems of low battery efficiency and short battery life in the prior art.
According to the technical scheme, the preparation method of the soft and hard double-layer lithium sulfur battery anode comprises the steps of preparing porous carbon powder from egg white, mixing the prepared porous carbon powder into slurry by using a polytetrafluoroethylene binder, coating the slurry on one side of a porous polypropylene film, and adhering a coating layer of the polypropylene film with the slurry to an original anode of a solid lithium sulfur battery to prepare the double-layer lithium sulfur battery anode, wherein the original anode of the lithium sulfur battery is solid, and the coated anode of the lithium sulfur battery is plastic, so that the soft and hard combined double-layer lithium sulfur battery anode is realized.
The present invention is also characterized in that,
the method is implemented according to the following steps:
step 2, adding 1.5-2.0wt% of polytetrafluoroethylene binder into the porous carbon powder prepared in the step 1, and uniformly stirring to obtain slurry;
step 3, brushing the slurry obtained in the step 2 on the surface of one side of the polypropylene net film, and then putting the polypropylene net film in a vacuum environment for a period of time to obtain the polypropylene net film with one conductive surface and the other insulating surface;
step 4, coating a polytetrafluoroethylene binder on the edge of the coated side of the polypropylene net film obtained in the step 3, and pasting a film on the surface of the original porous carbon sulfur anode of the sulfur lithium battery, wherein the insulating polypropylene film is arranged on the outer side of the anode of the sulfur lithium battery, so that the soft and hard double-layer sulfur lithium battery anode is obtained;
and 5, soaking the soft and hard double-layer lithium sulfur battery anode obtained in the step 4 in the lithium sulfur battery electrolyte, and installing the lithium sulfur battery on one side of the polypropylene film of the double-layer lithium sulfur battery anode facing to the cathode after the soft and hard double-layer lithium sulfur battery anode is saturated and adsorbs the electrolyte.
The stagnation time in step 1 is controlled to be 1-1.5 hours.
In the step 1, the temperature for freezing the foamed egg white is controlled to be-10-15 ℃, and the freezing time is 1-1.5 hours.
In the step 1, the obtained porous carbon material is ground to be less than 20-30 μm.
And 3, coating the surface of the polypropylene net film with the slurry to a thickness of 0.2-0.4mm.
In the step 3, the temperature of the vacuum environment is 50-60 ℃, and the polypropylene net film coated with the sizing agent is placed in the vacuum environment for 2-4 hours.
And 5, soaking the anode of the soft-hard double-layer sulfur lithium battery in the electrolyte of the sulfur lithium battery for at least 3 hours.
The preparation method of the soft-hard double-layer lithium sulfur battery anode has the advantages that the porous carbon powder material is coated on one side of the polypropylene, the porous carbon material is prepared from egg white and contains natural elements such as N, O and the like, the conductivity of the carbon material is improved due to the addition of N, the adsorption capacity of the surface of the carbon material is improved due to O, and sulfides can be easily adsorbed by the carbon material. Medical mask materialThe pore diameter of the filtered pores becomes smaller after the porous carbon powder is coated, so that Li can be effectively prevented 2 S 8 、Li 2 And the shuttling of substances such as S6 and the like can only enable Li ions with smaller radius in the lithium sulfur battery to pass through. When solid carbon-sulfur battery discharges, solid S-S discharges to produce liquid-phase Li 2 S 8 The volume of the solution expands, the small holes in the anode of the lithium sulfur battery are filled, part of the solution is discharged to enter the small holes, the discharged sulfide is blocked by the polypropylene film on the outer side, a crack is formed between the polypropylene film and the original porous carbon hard anode, and the discharged sulfide is still in the small holes, so that the polypropylene material has certain plasticity, and the defects that the porous material collapses, the anode interface is reduced and the discharge efficiency is lowered due to the volume expansion are effectively prevented; when sulfide flowing into the outside of the small hole is blocked by the carbon film on one side of the soft polypropylene, the carbon film has stronger adsorption capacity and adsorbs the sulfide on the surface of the film, thereby being beneficial to further discharging.
Drawings
Fig. 1 is a graph of rate performance tests performed on the soft and hard lithium sulfur battery anodes of the present invention at rates of 0.05C, 0.1C, 0.2C, 0.5C, 1C, and 2C, respectively.
Detailed Description
The present invention will be described in detail below with reference to the accompanying drawings and specific embodiments.
The invention relates to a preparation method of a soft and hard double-layer lithium sulfur battery anode, which comprises the steps of preparing porous carbon powder by egg white, mixing the prepared porous carbon powder into slurry by using a polytetrafluoroethylene binder, coating the slurry on one side of a porous polypropylene film, and adhering a coating layer of the polypropylene film with the slurry to an original solid lithium sulfur battery anode to prepare a two-layer lithium sulfur battery anode.
The method is implemented according to the following steps:
step 2, adding 1.5-2.0wt% of polytetrafluoroethylene binder into the porous carbon powder prepared in the step 1, and uniformly stirring to obtain slurry;
step 3, coating the surface of one side of the polypropylene net film with the slurry obtained in the step 2, wherein the coating thickness is 0.2-0.4mm, then placing the polypropylene net film in a vacuum environment for a period of time, the temperature of the vacuum environment is 50-60 ℃, and the polypropylene net film coated with the slurry is placed in the vacuum environment for 2-4 hours to obtain the polypropylene net film with one conductive surface and the other insulating surface;
step 4, coating a polytetrafluoroethylene binder on the edge of the coated side of the polypropylene net film obtained in the step 3, and pasting a film on the surface of the original porous carbon sulfur anode of the sulfur lithium battery, wherein the insulating polypropylene film is arranged on the outer side of the anode of the sulfur lithium battery, so that the soft and hard double-layer sulfur lithium battery anode is obtained;
and 5, soaking the soft and hard double-layer sulfur lithium battery anode obtained in the step 4 in the sulfur lithium battery electrolyte for at least 3 hours, and after the soft and hard double-layer sulfur lithium battery anode is saturated and adsorbs the electrolyte, mounting the sulfur lithium battery with one side of a polypropylene film of the double-layer sulfur lithium battery anode facing a cathode.
The invention pastes a layer of polypropylene porous membrane on the surface of the original porous carbon anode, the polypropylene porous membrane is a commercially available medical mask inner side material and contains smaller gaps, one side of the membrane is coated with a layer of porous carbon, the design can lead extruded sulfide to flow between two interlayers, the medical polypropylene material is a plastic material with elasticity, thus effectively preventing the collapse of the original porous carbon material due to volume expansion, the reticular polypropylene membrane prevents sulfide from flowing to a cathode, and the shuttle process is reduced, therefore, the invention effectively improves the current efficiency of the sulfur lithium battery and the service life of the battery.
Example 1
The invention relates to a preparation method of a soft and hard double-layer sulfur lithium battery anode, which is implemented according to the following steps:
step 2, adding 1.5wt% of polytetrafluoroethylene binder into the porous carbon powder prepared in the step 1, and uniformly stirring to obtain slurry;
step 3, coating the surface of one side of the polypropylene net film with the slurry obtained in the step 2, wherein the coating thickness is 0.2mm, and then placing the polypropylene net film in a vacuum environment for a period of time, wherein the temperature of the vacuum environment is 50 ℃, the polypropylene net film coated with the slurry is placed in the vacuum environment for 4 hours, so that the polypropylene net film with one conductive surface and the other insulating surface is obtained;
step 4, coating a polytetrafluoroethylene binder on the edge of the coated side of the polypropylene net film obtained in the step 3, and pasting a film on the surface of the original porous carbon sulfur anode of the sulfur lithium battery, wherein the insulating polypropylene film is arranged on the outer side of the anode of the sulfur lithium battery, so that the soft and hard double-layer sulfur lithium battery anode is obtained;
and 5, soaking the soft and hard double-layer sulfur lithium battery anode obtained in the step 4 in the sulfur lithium battery electrolyte for at least 3 hours, and after the soft and hard double-layer sulfur lithium battery anode is saturated and adsorbs the electrolyte, mounting the sulfur lithium battery with one side of a polypropylene film of the double-layer sulfur lithium battery anode facing a cathode.
Example 2
The invention relates to a preparation method of a soft and hard double-layer sulfur lithium battery anode, which is implemented according to the following steps:
step 2, adding 1.8wt% of polytetrafluoroethylene binder into the porous carbon powder prepared in the step 1, and uniformly stirring to obtain slurry;
step 3, coating the surface of one side of the polypropylene net film with the slurry obtained in the step 2, wherein the coating thickness is 0.3mm, then placing the polypropylene net film in a vacuum environment for a period of time, the temperature of the vacuum environment is 55 ℃, and the polypropylene net film coated with the slurry is placed in the vacuum environment for 3 hours to obtain the polypropylene net film with one conductive surface and the other insulating surface;
step 4, coating a polytetrafluoroethylene binder on the edge of the coated side of the polypropylene net film obtained in the step 3, and pasting a film on the surface of the original porous carbon sulfur anode of the sulfur lithium battery, wherein the insulating polypropylene film is arranged on the outer side of the anode of the sulfur lithium battery, so that the soft and hard double-layer sulfur lithium battery anode is obtained;
and 5, soaking the soft and hard double-layer lithium sulfur battery anode obtained in the step 4 in the electrolyte of the lithium sulfur battery for at least 3 hours, and after the soft and hard double-layer lithium sulfur battery anode is saturated and adsorbs the electrolyte, installing the lithium sulfur battery on the side, facing the cathode, of the polypropylene film of the double-layer lithium sulfur battery anode.
Example 3
The invention relates to a preparation method of a soft and hard double-layer sulfur lithium battery anode, which is implemented according to the following steps:
step 2, adding 2.0wt% of polytetrafluoroethylene binder into the porous carbon powder prepared in the step 1, and uniformly stirring to obtain slurry;
step 3, coating the surface of one side of the polypropylene net film with the slurry obtained in the step 2, wherein the coating thickness is 0.4mm, and then placing the polypropylene net film in a vacuum environment for a period of time, wherein the temperature of the vacuum environment is 60 ℃, and the polypropylene net film coated with the slurry is placed in the vacuum environment for 2 hours to obtain the polypropylene net film with one conductive surface and the other insulating surface;
step 4, coating a polytetrafluoroethylene binder on the edge of the side, containing the coating, of the polypropylene net film obtained in the step 3, and pasting a film on the surface of the porous carbon sulfur anode of the original sulfur lithium battery, wherein at the moment, the outer side of the anode of the sulfur lithium battery is an insulating polypropylene film, so that a soft and hard double-layer sulfur lithium battery anode is obtained;
and 5, soaking the soft and hard double-layer sulfur lithium battery anode obtained in the step 4 in the sulfur lithium battery electrolyte for at least 3 hours, and after the soft and hard double-layer sulfur lithium battery anode is saturated and adsorbs the electrolyte, mounting the sulfur lithium battery with one side of a polypropylene film of the double-layer sulfur lithium battery anode facing a cathode.
Effects of the implementation
The positive electrode of the soft and hard sulfur lithium battery of the invention is subjected to a rate performance test under the conditions that the rates are respectively 0.05C, 0.1C, 0.2C, 0.5C, 1C and 2C, and finally the rate performance test returns to 0.2C, and the result is shown in figure 1. The specific discharge capacity of the battery from 0.05C to 2C is 1647.69, 1420.55, 1150.46, 950.32, 823.21 and 703.69 mAh.g < -1 >, and the specific discharge capacity of the existing lithium sulfur battery anode at 0.05C, 0.1C, 0.2C, 0.5C, 1C and 2C is 1435.28, 1104.53, 873.55, 735.32, 652.45 and 556.40 mAh.g < -1 >. The discharge rate is obviously higher than that of an unmodified single anode. The high rate of 2C returns to 0.2C again, the specific discharge capacity of the button battery prepared by the invention is 939.13mAh & g < -1 >, the specific discharge capacity is 1014.46mAh & g < -1 > when the charge-discharge cycle is stable, while the button batteries assembled by single anodes are 746.221 and 805.75mAh & g < -1 > respectively, and the specific discharge capacity of the anode of the invention is improved by 25.90 percent compared with that of a single anode battery when the anode is stably cycled at 0.2C.
Claims (1)
1. A preparation method of a soft and hard double-layer lithium sulfur battery cathode is characterized in that porous carbon powder is prepared by egg white, the prepared porous carbon powder is stirred into slurry by polytetrafluoroethylene binder, then the slurry is coated on one side of a porous polypropylene film, a coating layer of the polypropylene film coated with the slurry is adhered to the cathode of an original solid lithium sulfur battery to prepare a double-layer lithium sulfur battery cathode, the original lithium sulfur battery cathode is solid, and the coated film cathode is plastic, so that the soft and hard combined double-layer lithium sulfur battery cathode is obtained;
the method is implemented according to the following steps:
step 1, preparing porous carbon powder: adding NaHCO into egg white 3 ，NaHCO 3 The concentration in egg white is 0.2-0.25mol/L, then the mixture is stirred evenly and stands for 1-1.5 hours to foam the egg white, then the foamed egg white is frozen at the temperature of-10 to-15 ℃ for 1-1.5 hours, and then the frozen egg white is put in N 2 Calcining in a protected environment at 650-700 ℃ for 40-45min to obtain a porous carbon material, and finally grinding the porous carbon material to be less than 30 mu m;
step 2, adding 1.5-2.0wt% of polytetrafluoroethylene binder into the porous carbon powder prepared in the step 1, and uniformly stirring to obtain slurry;
step 3, coating the surface of one side of the polypropylene net film with the slurry obtained in the step 2, wherein the coating thickness is 0.2-0.4mm, and then placing the polypropylene net film in a vacuum environment for 2-4 hours at the temperature of 50-60 ℃ to obtain the polypropylene net film with one conductive surface and the other insulating surface;
step 4, coating a polytetrafluoroethylene binder on the edge of the coated side of the polypropylene net film obtained in the step 3, and pasting the film on the surface of the original sulfur lithium battery porous carbon sulfur cathode, wherein the insulating polypropylene film is arranged on the outer side of the sulfur lithium battery cathode to obtain a soft and hard double-layer sulfur lithium battery cathode;
and 5, soaking the soft and hard double-layer lithium sulfur battery cathode obtained in the step 4 in the electrolyte of the lithium sulfur battery for at least 3 hours, and after the soft and hard double-layer lithium sulfur battery cathode adsorbs the electrolyte in a saturated mode, installing the lithium sulfur battery with the polypropylene film side of the double-layer lithium sulfur battery cathode facing the anode.
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