CN111354906A - Modified diaphragm for lithium-sulfur battery and preparation method thereof - Google Patents
Modified diaphragm for lithium-sulfur battery and preparation method thereof Download PDFInfo
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- H01M50/00—Constructional details or processes of manufacture of the non-active parts of electrochemical cells other than fuel cells, e.g. hybrid cells
- H01M50/40—Separators; Membranes; Diaphragms; Spacing elements inside cells
- H01M50/403—Manufacturing processes of separators, membranes or diaphragms
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- H01M50/40—Separators; Membranes; Diaphragms; Spacing elements inside cells
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- H01M50/40—Separators; Membranes; Diaphragms; Spacing elements inside cells
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- H01M50/449—Separators, membranes or diaphragms characterised by the material having a layered structure
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Abstract
The invention belongs to the technical field of lithium-sulfur batteries, and particularly relates to a modified diaphragm for a lithium-sulfur battery and a preparation method thereof. The modified membrane contains g-C3N4A/CNT composite material. The modified diaphragm is added with g-C3N4the/CNT composite material not only improves the performance of the diaphragm material, overcomes the defects of obvious shuttle effect of polysulfide, obvious volume expansion effect of the lithium-sulfur battery, unstable electrochemical performance of the battery and the like in the lithium-sulfur battery prepared by the prior art, but also simplifies the production process and reduces the production cost.
Description
Technical Field
The invention belongs to the technical field of lithium-sulfur batteries, and particularly relates to a modified diaphragm for a lithium-sulfur battery and a preparation method thereof.
Background
The energy is an important pillar for supporting the development of the modern society, and the high-efficiency energy storage system can bring great innovation to the society. Batteries are one of the main ways of storing energy, and the renewal of batteries brings great changes to the renewable energy industry, the electronic industry and the electric automobile industry. Under the vigorous promotion of the state, the yield of global electric automobiles and lithium electric bicycles keeps a high-speed growth state, and further, the continuous high-speed growth of power type lithium ion batteries is driven, so that the power type lithium ion batteries become a main driving force for the growth of the global lithium ion battery industry. The nation is to develop new energy and new energy automobiles into the national strategy as a breakthrough for breaking the restriction between energy and environment and realizing the new economic growth. With the rapid expansion of markets of electric vehicles, new energy peak shaving power stations and the like, lithium ion batteries have become the key research field of main countries and various large enterprises, and the technological innovation and industrialization pace of the lithium ion batteries are greatly accelerated.
The lithium-sulfur battery has the advantages of high theoretical capacity and energy density, rich raw materials, good environmental protection, low cost and the like, and is considered to be one of the novel high-performance batteries with the most development potential at present. The lithium-sulfur battery is mainly composed of a positive electrode material, an electrolyte, a separator and a negative electrode material. The elemental sulfur as the positive electrode has higher specific capacity, and in a lithium/sulfur (Li/S) battery, the theoretical specific capacity is up to 1675 mA.h/g, the theoretical specific energy is 2600Wh/kg, which is higher than that of LiCoO in the traditional lithium ion battery2The equivalent positive electrode material is 6 times higher. However, the charging and discharging process of the lithium-sulfur battery is a multi-electron reaction accompanied by a complicated phase inversion process. When electrochemical reaction occurs, the intermediate discharge product is dissolved in the electrolyte and circularly shuttled between the positive electrode and the negative electrode. The shuttle effect seriously affects the cycle performance and the coulombic efficiency of the lithium-sulfur battery, and causes the problems of serious self-discharge of the lithium-sulfur battery and the like.
In order to solve the above problems, studies have shown that the modification treatment of the battery separator can significantly inhibit the shuttling effect of polysulfide and can capture polysulfide, and the prior art improves the performance of lithium sulfur batteries to some extent, but has the general disadvantages: the electrochemical performance of the battery is unstable, and the specific capacity is not high enough; the shuttling effect of polysulfides remains significant; the volume expansion of the lithium-sulfur ion battery is remarkable; the experiment is complicated, the operation difficulty is large, and the production cost is high.
Disclosure of Invention
The invention aims to provide a modified diaphragm for a lithium-sulfur battery and a preparation method thereof, aiming at the defects, wherein g-C is added into the modified diaphragm3N4the/CNT composite material not only improves the diaphragm materialThe performance of the lithium sulfur battery overcomes the defects of obvious shuttle effect of polysulfide, obvious volume expansion effect of the lithium sulfur battery, unstable electrochemical performance of the battery and the like in the lithium sulfur battery prepared by the prior art, simplifies the production process and reduces the production cost.
The technical scheme of the invention is as follows: a modified diaphragm for lithium-sulfur battery contains g-C3N4A/CNT composite material.
The preparation method of the modified diaphragm for the lithium-sulfur battery comprises the following steps:
(1) preparation of graphitic carbon nitride g-C3N4And a suspension thereof: firstly, dissolving melamine in deionized water, and stirring until the melamine is completely dissolved to obtain a transparent melamine solution; then transferring the obtained melamine transparent solution into a reaction kettle for heating treatment, filtering and collecting a reaction product; finally, adding the reaction product into an alumina crucible, and calcining in air atmosphere; cooling to room temperature after completion, and collecting the final yellow product to obtain g-C3N4Powder; the obtained g-C3N4Adding deionized water into the powder, grinding to obtain g-C3N4A suspension;
(2) ultrasonic pulverization of g-C3N4Suspension: for g to C obtained in step (1)3N4The suspension is stirred and then is subjected to ultrasonic pulverization treatment to obtain g-C3N4Solution of the resulting g-C3N4Sealing the solution for later use;
(3) preparation of g-C3N4CNT mixed solution: g-C obtained in the step (2)3N4Mixing the solution and the carbon nano tube water dispersion solution for preparation, stirring the mixture firstly and then carrying out ultrasonic treatment after the preparation is finished to obtain g-C3N4a/CNT mixed solution;
(4) coating a diaphragm: firstly, g-C obtained in the step (3)3N4Drying the/CNT mixed solution to prepare g-C3N4And (3) adding NMP (N-methyl pyrrolidone) powder, grinding, coating on a clean diaphragm, and drying to obtain the modified diaphragm.
The heating treatment temperature in the step (1) is 145-185 ℃, and the heating time is 16-24 h; the calcination temperature is 400-520 ℃, and the calcination time is 2-4 h.
g-C prepared in the step (1)3N4The concentration of the suspension is 0.3-0.5 mg/mL.
The stirring time in the step (2) is 3-5 hours; the ultrasonic treatment specifically comprises the following steps: the ultrasonic time is 30-50 minutes; each sonication cycle time was 5 seconds, with 2 seconds sonication time and 3 seconds time intervals.
And (3) the mass fraction of the carbon nanotubes in the carbon nanotube aqueous dispersion in the step (3) is 10%.
G to C in the step (3)3N4g-C contained in the solution3N4The mass ratio of the carbon nanotubes to the carbon nanotubes contained in the carbon nanotube aqueous dispersion was 10: 1.
And (4) stirring for 3-5 hours in the step (3), and carrying out ultrasonic treatment for 3-5 hours.
And (4) dropwise adding the NMP in the step (4) in an amount of 2-4 mL.
The grinding time in the step (4) is 20-40 minutes; drying for 8-10 hours at 50 ℃.
The invention has the beneficial effects that: the modified diaphragm for the lithium-sulfur battery is added with g-C3N4/CNT，g-C3N4And the tubular structure of the CNT is beneficial to adsorbing polysulfide, the utilization rate of sulfur is improved, and the utilization of the CNT greatly enhances the conductivity of the material. Meanwhile, the preparation method of the modified diaphragm simplifies the production process and reduces the production cost.
Drawings
FIG. 1 shows g-C obtained in example 13N4SEM image of (d).
FIG. 2 shows g-C obtained in example 13N4SEM image of/CNT.
FIG. 3 shows g-C in example 13N4、CNT、g-C3N4XRD profile of/CNT.
Fig. 4 is an electrochemical charge-discharge curve of the modified separator respectively prepared in examples 1 to 3 for a lithium sulfur battery.
Detailed Description
The present invention will be described in detail below with reference to examples.
Example 1
The modified diaphragm for the lithium-sulfur battery contains g-C3N4A/CNT composite material.
The preparation method of the modified diaphragm for the lithium-sulfur battery comprises the following steps:
(1) preparation of graphitic carbon nitride g-C3N4And a suspension thereof: firstly, dissolving melamine in deionized water, and stirring until the melamine is completely dissolved to obtain a transparent melamine solution; then transferring the obtained melamine transparent solution into a reaction kettle for heating treatment for 16h at 145 ℃, filtering and collecting reaction products; finally, adding the reaction product into an alumina crucible, and calcining in air atmosphere at 400 ℃ for 2 h; cooling to room temperature after completion, and collecting the final yellow product to obtain g-C3N4Powder; 0.06g of g-C3N4Grinding the powder with deionized water to uniformity, transferring to a measuring cylinder, and adding deionized water to 200mL to obtain 0.3mg/mL g-C3N4A suspension;
(2) ultrasonic pulverization of g-C3N4Suspension: for g to C obtained in step (1)3N4Stirring the suspension for 3 hours by using a stirrer, and then placing the suspension in an ultrasonic cell crusher for ultrasonic treatment, wherein the ultrasonic time is 50 minutes; each ultrasonic cycle time is 5 seconds, wherein the ultrasonic time is 2 seconds, and the time interval is 3 seconds; to obtain g-C3N4Solution of the resulting g-C3N4Sealing the solution for later use;
(3) preparation of g-C3N4CNT mixed solution: adding 0.06g of 10 mass percent carbon nano tube water dispersion liquid into the g-C obtained in the step (2)3N4Adding into the solution, stirring for 5 hr in a stirrer, and ultrasonic treating for 3 hr to obtain g-C3N4a/CNT mixed solution;
(4) coating a diaphragm: firstly, g-C obtained in the step (3)3N4Drying the/CNT mixed solution to prepare g-C3N4CNT powder, then 0.06g of g-C3N4Mixing the CNT powder, 0.0075g of conductive agent Keqin black and 0.0075g of adhesive PVDF, dropwise adding 2ml of NMP, grinding for 30 minutes, finally coating on a clean diaphragm, and drying for 8 hours at 50 ℃ to obtain the modified diaphragm.
Pure sulfur is taken as a positive electrode material, metal lithium is taken as a counter electrode and a reference electrode, lithium sulfur electrolyte is added, the modified diaphragm obtained in the embodiment is taken as a diaphragm, and the CR2025 button cell is assembled in a glove box filled with argon.
As can be seen from FIG. 1, g-C3N4Is dispersed in a sheet shape, and is beneficial to the full combination with the carbon nano tube.
As can be seen from FIG. 2, g-C3N4After being compounded with CNT, the CNT is more uniformly dispersed in g-C3N4The above.
As can be seen from comparison of the XRD curves in fig. 3, the diffraction peak at 26.4 ° can be attributed to the graphite-like structure (002) of the carbon nanotube. Pure g-C3N4There are two distinct diffraction peaks at 13.0 ° and 27.2 ° that correspond to the graphitized material of the (100) and (002) diffraction planes of JCPDS 87-1526. g-C3N4The peak at 13.0 ℃ in the/CNT sample disappeared, the main peak at 27.2 ℃ was higher, further demonstrating g-C3N4Protonation has been successful. In g-C3N4No significant CNT diffraction peak was observed in the/CNT composite sample due to the loading of trace amounts of CNTs.
Example 2
The preparation method of the modified diaphragm for the lithium-sulfur battery comprises the following steps:
(1) preparation of graphitic carbon nitride g-C3N4And a suspension thereof: firstly, dissolving melamine in deionized water, and stirring until the melamine is completely dissolved to obtain a transparent melamine solution; then transferring the obtained melamine transparent solution into a reaction kettle, carrying out heating treatment for 20 hours at 165 ℃, filtering and collecting a reaction product; finally, adding the reaction product into an alumina crucible, calcining in air atmosphere, and calciningThe temperature is 460 ℃, and the calcining time is 3 h; cooling to room temperature after completion, and collecting the final yellow product to obtain g-C3N4Powder; 0.08g of g-C3N4Grinding the powder with deionized water to uniformity, transferring to a measuring cylinder, and adding deionized water to 200mL to obtain 0.4mg/mL g-C3N4A suspension;
(2) ultrasonic pulverization of g-C3N4Suspension: for g to C obtained in step (1)3N4Stirring the suspension for 3 hours by using a stirrer, and then placing the suspension in an ultrasonic cell crusher for ultrasonic treatment for 30 minutes; each ultrasonic cycle time is 5 seconds, wherein the ultrasonic time is 2 seconds, and the time interval is 3 seconds; to obtain g-C3N4Solution of the resulting g-C3N4Sealing the solution for later use;
(3) preparation of g-C3N4CNT mixed solution: adding 0.08g of 10 mass percent carbon nano tube aqueous dispersion into the g-C obtained in the step (2)3N4Adding into the solution, stirring for 3 hr in a stirrer, and ultrasonic treating for 4 hr to obtain g-C3N4a/CNT mixed solution;
(4) coating a diaphragm: firstly, g-C obtained in the step (3)3N4Drying the/CNT mixed solution to prepare g-C3N4The powder of/CNT was taken up in 0.08g of g-C3N4Mixing the CNT powder, 0.01g of conductive agent Ketjen black and 0.01g of adhesive PVDF, dropwise adding 3mLNMP, grinding for 30 minutes, finally coating on a clean diaphragm, and drying for 9 hours at 50 ℃ to obtain the modified diaphragm.
Example 3
The preparation method of the modified diaphragm for the lithium-sulfur battery comprises the following steps:
(1) preparation of graphitic carbon nitride g-C3N4And a suspension thereof: firstly, dissolving melamine in deionized water, and stirring until the melamine is completely dissolved to obtain a transparent melamine solution; then transferring the obtained melamine transparent solution into a reaction kettle for heating treatment for 24 hours at 185 ℃, filtering and collecting reaction products; finally, the reaction product is reactedAdding the mixture into an alumina crucible, and calcining the mixture in air atmosphere at the calcining temperature of 520 ℃ for 4 hours; cooling to room temperature after completion, and collecting the final yellow product to obtain g-C3N4Powder; 0.1g of g-C3N4Grinding the powder with deionized water to uniformity, transferring to a measuring cylinder, and adding deionized water to 200mL to obtain 0.5mg/mL g-C3N4A suspension;
(2) ultrasonic pulverization of g-C3N4Suspension: for g to C obtained in step (1)3N4Stirring the suspension for 5 hours by using a stirrer, and then placing the suspension in an ultrasonic cell crusher for ultrasonic treatment, wherein the ultrasonic time is 40 minutes; each ultrasonic cycle time is 5 seconds, wherein the ultrasonic time is 2 seconds, and the time interval is 3 seconds; to obtain g-C3N4Solution of the resulting g-C3N4Sealing the solution for later use;
(3) preparation of g-C3N4CNT mixed solution: adding 0.1g of 10 mass percent carbon nano tube aqueous dispersion into the g-C obtained in the step (2)3N4Adding into the solution, stirring for 5 hr in a stirrer, and ultrasonic treating for 5 hr to obtain g-C3N4a/CNT mixed solution;
(4) coating a diaphragm: firstly, g-C obtained in the step (3)3N4Drying the/CNT mixed solution to prepare g-C3N4The powder of/CNT was taken up in 0.1g of g-C3N4Mixing the/CNT powder, 0.0125g of conductive agent Keqin black and 0.0125g of adhesive PVDF, then dropwise adding 4ml of NMP to grind for 40 minutes, finally coating on a clean diaphragm, and drying for 10 hours at 50 ℃ to obtain the modified diaphragm.
As can be seen from the charge and discharge curves in fig. 4, in the case of example 3, the specific discharge capacity and the cycling stability of the lithium-sulfur battery were the best, and example 2 also had more excellent specific discharge capacity and cycling stability than example 1, which proves that the process parameters in the method are not obvious.
Claims (10)
1. Modified separator for lithium-sulfur batteryFilm, characterized in that the modified separator contains g-C3N4A/CNT composite material.
2. A method for preparing a modified separator for a lithium-sulfur battery according to claim 1, comprising the steps of:
(1) preparation of graphitic carbon nitride g-C3N4And a suspension thereof: firstly, dissolving melamine in deionized water, and stirring until the melamine is completely dissolved to obtain a transparent melamine solution; then transferring the obtained melamine transparent solution into a reaction kettle for heating treatment, filtering and collecting a reaction product; finally, adding the reaction product into an alumina crucible, and calcining in air atmosphere; cooling to room temperature after completion, and collecting the final yellow product to obtain g-C3N4Powder; the obtained g-C3N4Adding deionized water into the powder, grinding to obtain g-C3N4A suspension;
(2) ultrasonic pulverization of g-C3N4Suspension: for g to C obtained in step (1)3N4The suspension is stirred and then is subjected to ultrasonic pulverization treatment to obtain g-C3N4Solution of the resulting g-C3N4Sealing the solution for later use;
(3) preparation of g-C3N4CNT mixed solution: g-C obtained in the step (2)3N4Mixing the solution and the carbon nano tube water dispersion solution for preparation, stirring the mixture firstly and then carrying out ultrasonic treatment after the preparation is finished to obtain g-C3N4a/CNT mixed solution;
(4) coating a diaphragm: firstly, g-C obtained in the step (3)3N4Drying the/CNT mixed solution to prepare g-C3N4And (3) adding NMP (N-methyl pyrrolidone) powder, grinding, coating on a clean diaphragm, and drying to obtain the modified diaphragm.
3. The method for preparing the modified separator for the lithium-sulfur battery according to claim 2, wherein the heating treatment in the step (1) is carried out at a temperature of 145-185 ℃ for 16-24 h; the calcination temperature is 400-520 ℃, and the calcination time is 2-4 h.
4. The method for preparing a modified separator for a lithium-sulfur battery according to claim 2, wherein g-C prepared in the step (1)3N4The concentration of the suspension is 0.3-0.5 mg/mL.
5. The method for preparing the modified separator for the lithium-sulfur battery according to claim 2, wherein the stirring time in the step (2) is 3 to 5 hours; the ultrasonic treatment specifically comprises the following steps: the ultrasonic time is 30-50 minutes; each sonication cycle time was 5 seconds, with 2 seconds sonication time and 3 seconds time intervals.
6. The method for preparing a modified separator for a lithium-sulfur battery according to claim 4, wherein the mass fraction of carbon nanotubes in the aqueous dispersion of carbon nanotubes in the step (3) is 10%.
7. The method for preparing a modified separator for a lithium-sulfur battery according to claim 6, wherein g-C in the step (3)3N4g-C contained in the solution3N4The mass ratio of the carbon nanotubes to the carbon nanotubes contained in the carbon nanotube aqueous dispersion was 10: 1.
8. The method for preparing the modified separator for the lithium-sulfur battery according to claim 2, wherein the stirring time in the step (3) is 3 to 5 hours, and the ultrasonic treatment is performed for 3 to 5 hours.
9. The method for preparing a modified separator for a lithium-sulfur battery according to claim 2, wherein the amount of NMP added in step (4) is 2 to 4 mL.
10. The method for preparing the modified separator for a lithium-sulfur battery according to claim 2, wherein the grinding time in the step (4) is 20 to 40 minutes; drying for 8-10 hours at 50 ℃.
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