CN111864190B - Preparation method of flexible sulfur positive electrode of lithium-sulfur battery - Google Patents
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Abstract
The invention discloses a preparation method of a flexible sulfur positive electrode of a lithium-sulfur battery, and belongs to the technical field of lithium-sulfur batteries. The flexible sulfur positive electrode of the lithium sulfur battery comprises flexible multifunctional carbon foam and a sulfur-containing active substance loaded in the flexible multifunctional carbon foam, and the specific preparation process comprises the steps of preparation of the flexible multifunctional carbon foam, preparation of the flexible sulfur positive electrode of the lithium sulfur battery and the like. The synthesis method is simple and convenient to operate, low in cost, suitable for large-scale production and significant to large-scale production of lithium-sulfur batteries.
Description
Technical Field
The invention belongs to the technical field of lithium-sulfur batteries, and particularly relates to a preparation method of a flexible sulfur positive electrode of a lithium-sulfur battery.
Background
With the flourishing development of the fields of flexible and wearable electronic products, the development of an energy storage system with good flexibility, high energy density and long cycle life is urgently needed. In the current selection, the lithium-sulfur battery has a plurality of significant advantages of high theoretical specific capacity (1675 mAh/g) due to multi-electron conversion reaction, wide sulfur source of the positive active material, low price, environmental friendliness and the like, can meet the requirements of the consumer electronics market, and is a promising next-generation chemical power system. In particular, flexible lithium-sulfur batteries are very attractive, and their portability and applicability can be adapted to different application scenarios. However, lithium-sulfur batteries have not been commercialized yet because of their own non-negligible drawbacks. The reason is as follows: first, the insulation of sulfur and its discharge products; secondly, the polysulfide ions of the discharge intermediate product are dissolved in the electrolyte and the 'shuttle effect' is accompanied; third, the volume of sulfur expands in the electrochemical reaction. These disadvantages result in lower utilization of active materials, poor cycling stability and low coulombic efficiency of lithium-sulfur batteries, which severely limits the widespread use of lithium-sulfur batteries. In the case of high sulfur loadings, the above problem is exacerbated. However, the conventional sulfur composite positive electrode has problems of poor mechanical properties of an electrode, reduction of conductivity of a pole piece during bending or deformation, and the like besides problems of dissolution and shuttle effects of polysulfide inherent in a lithium sulfur battery, and the like, and influences the development and application of a flexible lithium sulfur battery. Therefore, new solutions for sulfur storage nanostructures must be designed to meet the requirements of flexible lithium-sulfur battery cell materials in terms of capacity, stability, flexibility, etc. at the same time.
The independently supported mixed positive electrode material is one of the development trends of flexible lithium-sulfur batteries and is a great hot spot of research nowadays. Currently, many attempts to improve sulfur loading have been made with three-dimensional current collectors, including aluminum foam, nickel foam, carbon nanotube paper, carbon fiber-based materials, graphene aerogel, and graphene foam, among others. The invention provides a three-dimensional carbon current collector of a lithium sulfur battery (Chinese invention patent, publication No. CN 105489901B) at the earlier stage of the subject group, which is characterized in that a cheap organic foaming material is carbonized at high temperature to prepare the three-dimensional carbon current collector, the three-dimensional carbon current collector has the performances of a conductive agent and an adsorbent, and the migration of polysulfide in electrolyte is effectively inhibited, so that the three-dimensional carbon current collector has the function of effectively fixing sulfur, the cycle stability of the lithium sulfur battery is improved, the surface sulfur carrying capacity of the current collector can be improved by the three-dimensional structure, and the three-dimensional carbon current collector has certain flexibility and can offset the volume expansion of sulfur in the charging and discharging process.
However, the pores of the three-dimensional carbon skeleton are too large and lack good short-range electron conductivity. In addition, due to the lack of strong polar substances which have strong polarity and can absorb and catalyze polysulfide conversion, the three-dimensional carbon material has limited capability of binding sulfur, and the rate capability also needs to be further improved. Therefore, the interface properties (conductivity and affinity) and the pore structure of the conductive polar skeleton of the flexible nanocarbon current collector which are reasonably regulated and controlled can promote the conversion of sulfur/polysulfide, and the method is an effective means for improving the high-efficiency work of the flexible sulfur positive electrode of the lithium-sulfur battery.
Disclosure of Invention
The invention provides a preparation method of a flexible sulfur positive electrode of a lithium sulfur battery, which comprises the steps of preparing a three-dimensional flexible carbon foam framework by taking polyurethane foam as a precursor, growing carbon nano tubes with short-range electronic conductivity and cobalt sulfide (Co) capable of chemically adsorbing and catalytically converting polysulfide on the three-dimensional flexible carbon foam framework in situ9S8) Finally obtaining flexible multifunctional carbon foam, and then loading the sulfur-containing active substance in the flexible multifunctional carbon foam to obtain the high-sulfur-loading-capacity flexible sulfur positive electrode of the lithium-sulfur battery.
The invention adopts the following technical scheme for solving the technical problems, and the preparation method of the flexible sulfur positive electrode of the lithium-sulfur battery is characterized in that the flexible sulfur positive electrode of the lithium-sulfur battery comprises flexible multifunctional carbon foam and a sulfur-containing active substance loaded in the flexible multifunctional carbon foam, and the specific preparation process comprises the following steps:
step S1: preparing flexible multifunctional carbon foam, namely soaking polyurethane foam into an organic solvent, washing and drying by ultrasonic, soaking the dried polyurethane foam into an ethanol solution of metal cobalt salt and a sulfur source, stirring or performing ultrasonic treatment until the metal cobalt salt and the sulfur source are fully soaked, heating to 450-DEG C and 600-DEG C in an inert atmosphere, preserving heat for 2h, heating to 800-DEG C and 900-DEG C, preserving heat for 2h, and naturally cooling to room temperature to prepare the flexible multifunctional carbon foam, wherein the flexible multifunctional carbon foam comprises a carbon foam framework and a carbon nano tube/cobalt sulfide component growing in situ on the carbon foam framework, the metal cobalt salt is at least one of cobalt nitrate, cobalt acetate or cobalt chloride, and the metal sulfur source is any one of elemental sulfur, thiourea or thioacetamide;
step S2: preparing a flexible sulfur anode of the lithium-sulfur battery, namely soaking the flexible multifunctional carbon foam prepared in the step S1 into elemental sulfur dispersion liquid with the concentration of 10-30mg/mL, standing and drying the elemental sulfur dispersion liquid in which the solvent is toluene or carbon disulfide, placing the mixture into a closed container, and preserving the heat for 10-28h at the temperature of 180 ℃ in an inert atmosphere; or directly mixing the flexible multifunctional carbon foam prepared in the step S1 with elemental sulfur, then placing the mixture into a closed container, and preserving the heat for 10-28h at the temperature of 180 ℃ in an inert atmosphere, thus finally preparing the flexible sulfur positive electrode of the lithium-sulfur battery, wherein the flexible sulfur positive electrode of the lithium-sulfur battery is directly used for assembling the lithium-sulfur battery without being mixed with a conductive agent and a binder, and the energy density of the electrode is obviously improved while the working procedures are saved.
Preferably, the polyurethane foam in step S1 is melamine foam, and the organic solvent is any one of ethanol, ethylene glycol, isopropanol or acetone.
Preferably, the feeding ratio of the polyurethane foam and the metal cobalt salt in the step S1 is 1g:2.5mmol-1g:10mmol, and the feeding molar ratio of the metal cobalt salt to the sulfur source is 1:2.7-1: 6.6.
Preferably, the stirring or ultrasonic time for dipping in step S1 is 30min-24 h.
Preferably, in the step S1, the temperature is raised to 500-.
Preferably, the temperature increase rate of the calcination process in step S1 is 1-5 ℃/min, preferably 3 ℃/min, which helps to maintain the stability of the porous structure of the flexible multifunctional carbon foam.
The structure and composition of the flexible multifunctional carbon foam of the present invention have the following advantages: 1. the porous nanostructures inside the flexible multifunctional carbon foam provide large spaces to provide high sulfur loading and accommodate volumetric expansion of sulfur; 2. the conductivity of the flexible multifunctional carbon foam is high locally and integrally, wherein the carbon foam framework and the criss-cross three-dimensional conductive network of the carbon nano tubes can reduce the internal resistance and improve the utilization rate of sulfur; 3. the chemical adsorption and physical limitation of the flexible multifunctional carbon foam to polysulfide substances can effectively inhibit the shuttle effect; 4. the electrocatalytic effect of cobalt sulfide in the flexible multifunctional carbon foam promotes the redox conversion of sulfur species. The synthesis method is simple and convenient to operate, low in cost, suitable for large-scale production and significant to large-scale production of lithium-sulfur batteries.
Drawings
FIG. 1 is an optical photograph of a multifunctional carbon foam and precursor (left) and bend (right);
FIG. 2 is a scanning electron micrograph of flexible multifunctional carbon foam;
FIG. 3 is an XRD pattern of a flexible multifunctional carbon foam;
FIG. 4 is a graph of 0.5C cycle performance of the lithium sulfur batteries of example 1, example 2, and comparative example;
FIG. 5 is a graph of cycle performance of 1C of the lithium sulfur batteries of example 1, example 2, and comparative example;
fig. 6 is a charge-discharge graph of 0.5C of the lithium sulfur battery of example 1.
Detailed Description
The present invention is described in further detail below with reference to examples, but it should not be construed that the scope of the above subject matter of the present invention is limited to the following examples, and that all the technologies realized based on the above subject matter of the present invention belong to the scope of the present invention.
Example 1
The preparation method of the flexible multifunctional carbon foam of the embodiment comprises the following steps: using melamine foamSoaking in glycol for 6h, performing ultrasonic treatment for 0.5h, washing with distilled water for 3 times, drying in vacuum drying oven at 60 deg.C for 12h to obtain carbon precursor, soaking in 100mL solution containing 1mM Co (NO)3)2·6H2And (2) uniformly stirring O and 1g of thiourea in ethanol solution, carrying out ultrasonic treatment until the mixture is fully soaked, heating to 550 ℃ at the heating rate of 3 ℃/min in nitrogen atmosphere, keeping the temperature for 2h, heating to 800 ℃ and keeping the temperature for 2h, and naturally cooling to room temperature to obtain the flexible multifunctional carbon foam.
The preparation method of the positive electrode of the lithium-sulfur battery of the embodiment comprises the following steps: mixing the prepared flexible multifunctional carbon foam and elemental sulfur powder according to the mass ratio of 1:3, putting the mixture into a vacuumized closed reaction kettle, and preserving the heat for 10 hours at 155 ℃ in a nitrogen atmosphere to obtain the flexible sulfur anode of the lithium-sulfur battery, wherein the surface loading of the anode is 6mg/m2。
After the flexible sulfur electrode of the lithium-sulfur battery is assembled into the lithium-sulfur battery, the first discharge specific capacity of 846.6mAh/g is achieved, the cycle performance is excellent, and the capacity can be maintained at 712.5mAh/g after 200 cycles.
Example 2
The preparation method of the flexible multifunctional carbon foam of the embodiment comprises the following steps: soaking melamine foam in acetone for 3h, performing ultrasonic treatment for 0.5h, washing with distilled water for 3 times, drying in vacuum drying oven at 120 deg.C for 8h to obtain carbon precursor, soaking in 50mL of solution containing 4mM CoCl2·6H2And (2) stirring the mixture evenly in an ethanol solution of O and 2g thioacetamide, carrying out ultrasonic treatment until the mixture is fully soaked, heating to 500 ℃ at the heating rate of 3 ℃/min in a nitrogen atmosphere, keeping the temperature for 1h, heating to 850 ℃ and keeping the temperature for 0.5h, and naturally cooling to room temperature to obtain the flexible multifunctional carbon foam.
The preparation method of the positive electrode of the lithium-sulfur battery of the embodiment comprises the following steps: soaking the prepared flexible multifunctional carbon foam into a carbon disulfide solution with elemental sulfur concentration of 25mg/mL, standing overnight, drying, placing into a closed container, and preserving heat for 24 hours at 155 ℃ in a nitrogen atmosphere; then drying at 50 ℃, heating at 200 ℃ for 2h in nitrogen atmosphere to evaporate sulfur on the carbon surface, naturally cooling to room temperature to obtain the flexible sulfur positive electrode of the lithium-sulfur battery, wherein the positive electrode has the surface capacity of 10 mg/bamboom2。
The flexible sulfur electrode of the lithium-sulfur battery has the specific discharge capacity of 828mAh/g for the first time after being assembled into the lithium-sulfur battery, the cycle performance is excellent, and the capacity can be maintained at 608.8mAh/g after 200 cycles.
The comparative example is carbon foam obtained by directly heating melamine foam to 800 ℃ in nitrogen atmosphere and preserving heat for 2 hours, the preparation conditions of the positive electrode of the lithium-sulfur battery based on the carbon foam are the same as the preparation method of the flexible sulfur positive electrode of the lithium-sulfur battery in example 2, and the surface loading of the positive electrode is 4mg/m2. After the lithium-sulfur battery electrode is assembled into a lithium-sulfur battery, the first discharge specific capacity of 642mAh/g is obtained, and the capacity is attenuated to 334.7mAh/g after the lithium-sulfur battery electrode is cycled for 200 times.
As can be seen from fig. 4 and 5, the lithium sulfur battery obtained by the technical scheme of the present invention has greatly improved specific capacity and cycle stability, which indicates that the flexible multifunctional carbon foam of the present invention can effectively inhibit the dissolution of polysulfide in the electrolyte during the charging and discharging process, reduce the corrosion of polysulfide to the metal lithium cathode, and promote the conversion of polysulfide, thereby improving the cycle stability and rate capability of the lithium sulfur battery, and has important significance for realizing the production of high-performance flexible lithium sulfur batteries.
The foregoing embodiments illustrate the principles, principal features and advantages of the invention, and it will be understood by those skilled in the art that the invention is not limited to the foregoing embodiments, which are merely illustrative of the principles of the invention, and that various changes and modifications may be made therein without departing from the scope of the principles of the invention.
Claims (6)
1. A preparation method of a flexible sulfur positive electrode of a lithium sulfur battery is characterized in that the flexible sulfur positive electrode of the lithium sulfur battery comprises flexible multifunctional carbon foam and a sulfur-containing active substance loaded in the flexible multifunctional carbon foam, and the specific preparation process comprises the following steps:
step S1: the preparation of flexible multifunctional carbon foam includes soaking polyurethane foam in organic solvent, ultrasonic washing and drying, and soaking the dried polyurethane foam in metal cobalt salt and sulfur sourceStirring or ultrasonic treating the solution until the cobalt salt and the sulfur source are fully soaked, heating to 450-plus-one temperature for 600 h and preserving the heat for 2h in an inert atmosphere, heating to 800-plus-one temperature for 900 h and preserving the heat for 2h, and naturally cooling to room temperature to prepare the flexible multifunctional carbon foam, wherein the flexible multifunctional carbon foam comprises a carbon foam framework and a carbon nano tube/cobalt sulfide Co growing in situ on the carbon foam framework9S8The component comprises at least one of cobalt nitrate, cobalt acetate or cobalt chloride as the metal cobalt salt, and any one of thiourea or thioacetamide as the sulfur source;
step S2: preparing a flexible sulfur anode of the lithium-sulfur battery, namely soaking the flexible multifunctional carbon foam prepared in the step S1 into elemental sulfur dispersion liquid with the concentration of 10-30mg/mL, standing and drying the elemental sulfur dispersion liquid in which the solvent is toluene or carbon disulfide, placing the mixture into a closed container, and preserving the heat for 10-28h at the temperature of 180 ℃ in an inert atmosphere; or directly mixing the flexible multifunctional carbon foam prepared in the step S1 with elemental sulfur, then placing the mixture into a closed container, and preserving the heat for 10-28h at the temperature of 180 ℃ in an inert atmosphere, thus finally preparing the flexible sulfur positive electrode of the lithium-sulfur battery, wherein the flexible sulfur positive electrode of the lithium-sulfur battery is directly used for assembling the lithium-sulfur battery without being mixed with a conductive agent and a binder, and the energy density of the electrode is obviously improved while the working procedures are saved.
2. The method of preparing a flexible sulfur positive electrode for a lithium sulfur battery according to claim 1, wherein: in step S1, the polyurethane foam is melamine foam, and the organic solvent is any one of ethanol, ethylene glycol, isopropanol, and acetone.
3. The method of preparing a flexible sulfur positive electrode for a lithium sulfur battery according to claim 1, wherein: in the step S1, the feeding ratio of the polyurethane foam to the metal cobalt salt is 1g:2.5mmol-1g:10mmol, and the feeding molar ratio of the metal cobalt salt to the sulfur source is 1:2.7-1: 6.6.
4. The method of preparing a flexible sulfur positive electrode for a lithium sulfur battery according to claim 1, wherein: and in the step S1, stirring or ultrasonic treatment is carried out for 30min-24 h.
5. The method of preparing a flexible sulfur positive electrode for a lithium sulfur battery according to claim 1, wherein: in the step S1, the temperature is raised to 500-550 ℃ in the inert atmosphere and is preserved for 2h, then the temperature is raised to 800-850 ℃ and is preserved for 2h to prepare the flexible multifunctional carbon foam, and the calcination temperature and the preservation time are favorable for calcination to obtain the in-situ carbon nanotube/cobalt sulfide Co with excellent performance9S8Modified flexible multifunctional carbon foam and helps to maintain the integrity of the porous structure.
6. The method of making a flexible sulfur positive electrode for a lithium sulfur battery of claim 1, wherein: the temperature rise rate in the calcination process in the step S1 is 1-5 ℃/min, which is helpful for maintaining the stability of the flexible multifunctional carbon foam porous structure.
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