CN112670507A - Preparation method of lithium-sulfur battery intermediate layer of metal selenide-loaded carbon nanofiber and lithium-sulfur battery - Google Patents
Preparation method of lithium-sulfur battery intermediate layer of metal selenide-loaded carbon nanofiber and lithium-sulfur battery Download PDFInfo
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Abstract
The invention discloses a preparation method of a lithium-sulfur battery interlayer of metal selenide loaded carbon nanofibers and a lithium-sulfur battery, wherein an electrostatic spinning method is used for preparing a nanofiber membrane precursor: mixing metal acetate and Se powder in a certain proportion in N, N-dimethylformamide to obtain a solution A; dissolving polyacrylonitrile in N, N-dimethylformamide to obtain a solution B, mixing and stirring the A, B two solutions to prepare an electrostatic spinning solution, and carrying out electrostatic spinning by using the electrostatic spinning solution to finally obtain a nanofiber membrane of a metal selenide precursor; the carbon nanofiber membrane loaded with the metal selenide is prepared by a thermal annealing method. The carbon nanofiber membrane loaded with the metal selenide prepared by the method is applied to a lithium-sulfur battery as an intermediate layer, can enhance the adsorption catalysis effect on polysulfide, effectively adsorb and prevent polysulfide dissolved in electrolyte from migrating to a lithium cathode, and promote redox reaction in the charging and discharging processes of the lithium-sulfur battery, so that the rate capability and the cycling stability of the lithium-sulfur battery are effectively improved.
Description
Technical Field
The invention belongs to the technical field of lithium-sulfur batteries, and particularly relates to a preparation method of a carbon nanofiber lithium-sulfur battery interlayer loaded by metal selenide and a lithium-sulfur battery.
Background
With the rapid development of electronic portable devices and the electric automobile industry, the demand of the new energy market for electrochemical energy storage devices is increasing. Among them, lithium ion batteries are the most widely used energy storage devices in the market due to their excellent stability and power density, but have high cost and specific capacity (300mAh g)-1) The defects of low and the like are increasingly unable to meet the living needs of people. Therefore, the development of energy storage devices with high power density, high energy density and low cost is a hot spot of current research.
The elemental sulfur of the lithium-sulfur battery is used as a positive electrode material and has higher theoretical specific capacity (1675 mAh.g)-1) And theoretical energy density (2600Wh/Kg), and in addition elemental sulfur is inexpensive and environmentally friendly, so lithium sulfur batteries are one of the most promising rechargeable batteries at present.
Although lithium sulfur batteries have many advantages, three disadvantages of sulfur itself limit their practical applications: (1) insulation of sulfur: S/Li2The poor intrinsic conductivity of S hinders the utilization of the active material, resulting in low specific discharge capacity and low rate performance. In addition, the slow conduction of electrons and ions causes the lithium sulfur voltage plateau curve to tend to show greater polarization at lower discharge plateaus, further reducing the practical energy density of the lithium sulfur battery. (2) Shuttle effect: polysulfide (Li)2SnAnd n is more than or equal to 4 and less than or equal to 8) is easy to dissolve in the electrolyte solution, so that a shuttle effect exists between the anode and the cathode. Wherein shuttle of soluble polysulphides to the negative electrode forms insoluble Li2S, resulting in irreversible loss of the active material and low charging efficiency. (3) Volume expansion:sulfur formation of insoluble Li during charging2And S, the density of which is less than that of sulfur, so that the volume expansion of the lithiated electrode is caused, the maximum volume expansion rate can reach 80%, and finally the electrode material falls off.
To address these deficiencies, researchers have taken a number of measures to improve the performance of lithium sulfur batteries. For example, improvements are made in terms of positive electrode materials, separators, intermediate layers, electrolytes, and the like. However, merely improving the shuttle effect by physical and chemical adsorption does not solve the problem at all, and therefore the most effective solution is to catalytically promote the conversion of lithium polysulphides into solid Li2S2/Li2S to reduce its dissolution in the electrolyte. Thereby remarkably improving the cycle performance and rate performance of the lithium-sulfur battery.
Disclosure of Invention
In order to solve the defects in the prior art, the invention provides a preparation method of a metal selenide loaded carbon nanofiber lithium sulfur battery intermediate layer and a lithium sulfur battery provided with the intermediate layer, wherein the intermediate layer material of the lithium sulfur battery adopts metal selenide loaded carbon nanofiber, so that the adsorption catalysis effect on polysulfide can be enhanced, polysulfide dissolved in electrolyte is effectively prevented from migrating to a lithium cathode by adsorption, and the redox reaction in the charging and discharging processes of the polysulfide is promoted, so that the rate capability and the cycle stability of the lithium sulfur battery are effectively improved.
The technical scheme adopted by the invention is as follows:
the preparation method of the lithium-sulfur battery intermediate layer of the carbon nanofiber loaded by the metal selenide comprises the following steps:
s1, preparing a nanofiber membrane precursor by an electrostatic spinning method: mixing metal acetate and Se powder in a certain proportion in N, N-dimethylformamide to obtain a solution A; dissolving polyacrylonitrile in N, N-dimethylformamide to obtain a solution B, and mixing and stirring A, B two solutions to obtain an electrostatic spinning solution;
s2, carrying out electrostatic spinning on the electrostatic spinning solution to finally obtain a nanofiber membrane of the metal selenide precursor;
and S3, preparing the carbon nanofiber membrane loaded with the metal selenide by using a thermal annealing method.
Further, the metal acetate is Co (AC)2、Mo(AC)2Or Mn (AC)2；
Further, preparing metal acetate and Se powder in the mass ratio of (1-3): 1 in S1;
further, the parameters of the S2 electrospinning are set as follows: the working voltage is 12-15 kV, the translation distance is 100-130 mm, the injection rate is 0.08-0.1 mm/min, and the spinning distance is 20-25 cm.
Further, heating the nanofiber membrane prepared in the step S2 to 250-300 ℃ at a heating rate of 2-5 ℃/min in an air atmosphere, and preserving heat for pre-oxidation; and after cooling, heating the nanofiber membrane to 500-700 ℃ at a heating rate of 5-10 ℃/min in a nitrogen atmosphere, preserving heat, carbonizing and selenizing to obtain the metal selenide loaded carbon nanofiber membrane, and cutting the carbon nanofiber membrane by using a slicer to obtain the intermediate layer material of the lithium-sulfur battery.
The lithium-sulfur battery comprises a positive electrode, an intermediate layer, a diaphragm and a negative electrode, wherein the positive electrode, the intermediate layer, the diaphragm and the negative electrode are sequentially assembled in an argon atmosphere, and an electrolyte is added; the intermediate layer is the intermediate layer of the metal selenide-supported carbon nanofiber prepared by the method.
Further, the method for preparing the cathode material comprises the following steps: the CMK-3 and the sulfur powder with the mass ratio of 3:7 are subjected to heat preservation for 12 hours at the temperature of 155 ℃ by a melting method to prepare a sulfur composite material; preparing a sulfur composite material into slurry containing a conductive agent, a bonding agent and an organic solvent; coating the slurry on an aluminum foil current collector to serve as a positive pole piece of the lithium-sulfur battery, wherein the surface loading capacity is 1mg/cm2。
Further, the mass ratio of the sulfur composite material to the conductive agent to the adhesive is 7: 2: 1.
the invention has the beneficial effects that:
from the material aspect: the metal selenide has excellent catalytic action and adsorption capacity, and the transition metal has strong catalytic action, so that soluble polysulfide can be anchored and adsorbed in the charging and discharging process to prevent the soluble polysulfide from migrating to a lithium cathode, and the shuttle effect of the polysulfide is effectively improved. And strong catalytic property promotes the conversion of polysulfide in the charge-discharge process, and enhances the redox reaction degree in the cycle process. And the carbon nanofiber structure can enhance the conductivity of the lithium-sulfur battery, so that the lithium-sulfur battery has good reaction kinetics and electrochemical performance.
From the aspect of morphology: in the interlayer material, the carbon nano fibers form a mutually crossed net structure, and the metal selenide nano particles are uniformly dispersed on the surfaces of the carbon nano fibers, are uniform in appearance and are dispersed, so that more metal active sites are exposed, and Li (lithium) in the discharging process2S/Li2S2Uniform nucleation on the surface thereof, thereby improving the utilization rate of the active material and obtaining excellent electrochemical properties.
Drawings
FIG. 1 is a scanning electron micrograph of an interlayer material prepared in example 1;
FIG. 2 is an X-ray diffraction pattern of an interlayer material prepared in example 1;
FIG. 3 is a graph of rate performance of a lithium sulfur cell assembled with an interlayer material prepared in example 1;
fig. 4 is a graph of long cycle performance of a lithium sulfur battery assembled from example 1 and comparative example materials.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is described in further detail below with reference to the accompanying drawings and embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
Example 1
The preparation method of the lithium-sulfur battery intermediate layer of the carbon nanofiber loaded by the metal selenide comprises the following steps:
s1, preparation Co (AC)2Se/PAN electrospinning solution: first 4.5g Co (AC)2Mixing 1.5g Se powder with 2mL DMF solvent, stirring for 12h to obtain solution A, mixing 0.5g PAN with 5mL DMF solvent, stirring for 12h to obtain solution B, mixing solution A and solution B at 60 deg.C, stirring for 12h to obtain Co (AC)2-Se/PAN electrospinning solution;
s2 Synthesis of Co (AC) by electrospinning)2Se/PAN nanofiber membranes: performing electrostatic spinning on the prepared electrostatic spinning solution, wherein the working voltage is set to be 15kV, the injection rate is 0.1mm/min, the translation distance is 120mm, and the distance is set to be 25cm, so as to obtain Co (AC)2Se/PAN nanofibrous membranes.
S3, preparing a CoSe @ NC nanofiber membrane by a thermal annealing method: first, Co (AC)2And (3) raising the temperature of the-Se/PAN nanofiber membrane to 250 ℃ at the speed of 2 ℃/min in the air atmosphere, and preserving the temperature for 2h for pre-oxidation. And then heating the preoxidized nanofiber membrane to 550 ℃ at the speed of 5 ℃/min in the nitrogen atmosphere, preserving the heat for 3 hours, carbonizing and selenizing to obtain the CoSe @ NC nanofiber membrane, and cutting the CoSe @ NC nanofiber membrane into an intermediate layer material with the diameter of 14mm by using a slicing machine.
FIG. 1 is a scanning electron micrograph of the CoSe @ NC interlayer prepared in example 1 at high magnification. It can be seen that the material has a network of nanofibers with a diameter of 200mm crossing each other and surface-loaded with uniformly sized nanoparticles.
Fig. 2 is an X-ray diffraction pattern of the CoSe @ NC interlayer prepared in example 1, and it can be seen that this material has amorphous carbon and CoSe, i.e., a CoSe-supported carbon nanofiber material was prepared.
Fig. 3 is a graph of rate performance of a lithium sulfur cell assembled with a CoSe @ NC interlayer prepared in example 1, and it can be seen that this material has excellent rate performance.
Example 2
The preparation method of the lithium-sulfur battery intermediate layer of the carbon nanofiber loaded by the metal selenide comprises the following steps:
s1, preparation of Mo (AC)2Se/PAN electrospinning solution: firstly 4.5g Mo (AC)2Mixing 1.5g Se powder with 2mL DMF solvent, stirring for 12h to obtain solution A, mixing 0.5g PAN with 5mL DMF solvent, stirring for 12h to obtain solution B, mixing solution A and solution B at 60 deg.C, stirring for 12h to obtain Mo (AC)2-Se/PAN electrospinning solution;
s2 Synthesis of Mo (AC) by electrospinning2Se/PAN nanofiber membranes: carrying out electrostatic spinning on the prepared electrostatic spinning solution, wherein the working voltage is set to be 15kV, the injection rate is 0.1mm/min, the translation distance is 120mm, the distance is set to be 25cm,to obtain Mo (AC)2Se/PAN nanofibrous membranes.
S3, preparing the MoSe @ NC nanofiber membrane by a thermal annealing method: firstly, Mo (AC)2And (3) raising the temperature of the-Se/PAN nanofiber membrane to 250 ℃ at the speed of 2 ℃/min in the air atmosphere, and preserving the temperature for 2h for pre-oxidation. And then heating the preoxidized nanofiber membrane to 550 ℃ at the speed of 5 ℃/min in the nitrogen atmosphere, preserving the heat for 3 hours for carbonization and selenization to obtain the MoSe @ NC nanofiber membrane, and cutting the MoSe @ NC nanofiber membrane into an intermediate layer material with the diameter of 14mm by using a slicing machine.
Example 3
The preparation method of the lithium-sulfur battery intermediate layer of the carbon nanofiber loaded by the metal selenide comprises the following steps:
s1 preparation of Mn (AC)2Se/PAN electrospinning solution: first 4.5g Mn (AC)2Mixing 1.5g Se powder with 2mL DMF solvent, stirring for 12h to obtain solution A, mixing 0.5g PAN with 5mL DMF solvent, stirring for 12h to obtain solution B, mixing solution A and solution B at 60 deg.C, stirring for 12h to obtain Mn (AC)2-Se/PAN electrospinning solution;
s2 Synthesis of Mn (AC) by electrospinning2Se/PAN nanofiber membranes: performing electrostatic spinning on the prepared electrostatic spinning solution, wherein the working voltage is set to be 13kV, the injection rate is 0.1mm/min, the translation distance is 120mm, the distance is set to be 25cm, and Mn (AC) is obtained2Se/PAN nanofibrous membranes.
S3, preparing a MnSe @ NC nanofiber membrane by a thermal annealing method: firstly, Mn (AC)2And (3) raising the temperature of the-Se/PAN nanofiber membrane to 250 ℃ at the speed of 2 ℃/min in the air atmosphere, and preserving the temperature for 2h for pre-oxidation. And then heating the pre-oxidized nanofiber membrane to 550 ℃ at the speed of 5 ℃/min under the nitrogen atmosphere, preserving the heat for 3 hours, carbonizing and selenizing to obtain the MnSe @ NC nanofiber membrane, and cutting the MnSe @ NC nanofiber membrane into an intermediate layer material with the diameter of 14mm by using a slicing machine.
The application also designs a lithium-sulfur battery which comprises a positive electrode, a middle layer, a diaphragm and a negative electrode, wherein the positive electrode, the middle layer, the diaphragm and the negative electrode are sequentially assembled in an argon atmosphere, and 40 mu L of electrolyte is added(ii) a The intermediate layer is the intermediate layer of the metal selenide-supported carbon nanofiber prepared by the above method. The method for manufacturing the anode comprises the following steps: and (3) performing heat preservation on the CMK-3 and the sulfur powder in a mass ratio of 3:7 at 155 ℃ for 12 hours by using a melting method to prepare the sulfur composite material. The sulfur composite material was made into a slurry containing a conductive agent (Super P), a binder (PVDF), and an organic solvent (NMP). Wherein the mass ratio of the sulfur composite material to the conductive agent to the adhesive is 7: 2: 1, coating the slurry on an aluminum foil current collector to serve as a positive pole piece of the lithium-sulfur battery, wherein the surface loading is 1mg/cm2。
Comparative example 1
Comparative example 1 differs from example 1 in that: the remaining preparation method and conditions were the same as in example 1 without adding the interlayer material.
Comparative example 2
Comparative example 2 differs from example 1 in that: interlayer Material without Addition of Co (AC)2And Se powder, the other preparation method and conditions are the same as in example 1. Combining the long cycle performance profiles of the lithium sulfur cell assembled from example 1 and the comparative example material shown in fig. 4, it can be seen that the CoSe @ NC interlayer of example 1 possessed 823mAh g after 100 cycles at 0.1C-1Compared with the comparative example, the specific capacity of the catalyst obviously improves the cycling stability. Therefore, the metal selenide supported carbon nanofiber interlayer material prepared by the invention has excellent electrochemical performance.
The above embodiments are only used for illustrating the design idea and features of the present invention, and the purpose of the present invention is to enable those skilled in the art to understand the content of the present invention and implement the present invention accordingly, and the protection scope of the present invention is not limited to the above embodiments. Therefore, all equivalent changes and modifications made in accordance with the principles and concepts disclosed herein are intended to be included within the scope of the present invention.
Claims (8)
1. The preparation method of the lithium-sulfur battery intermediate layer of the carbon nanofiber loaded by the metal selenide is characterized by comprising the following steps of:
s1, preparing a nanofiber membrane precursor by an electrostatic spinning method: mixing metal acetate and Se powder in a certain proportion in N, N-dimethylformamide to obtain a solution A; dissolving polyacrylonitrile in N, N-dimethylformamide to obtain a solution B, and mixing and stirring A, B two solutions to obtain an electrostatic spinning solution;
s2, carrying out electrostatic spinning by using the electrostatic spinning solution to finally obtain the nanofiber membrane of the metal selenide precursor;
and S3, preparing the carbon nanofiber membrane loaded with the metal selenide by using a thermal annealing method.
2. The method for preparing an interlayer of a lithium-sulfur battery comprising metal selenide-supported carbon nanofibers according to claim 1, wherein the metal acetate is Co (AC)2、Mo(AC)2Or Mn (AC)2。
3. The method for preparing the intermediate layer of the metal selenide-supported carbon nanofiber lithium-sulfur battery as claimed in claim 2, wherein the metal acetate and the Se powder are arranged in a mass ratio of (1-3): 1 in S1.
4. The method for preparing an interlayer of a lithium-sulfur battery comprising metal selenide-supported carbon nanofibers according to claim 1, wherein the parameters of the S2 electrospinning are set as follows: the working voltage is 12-15 kV, the translation distance is 100-130 mm, the injection rate is 0.08-0.1 mm/min, and the spinning distance is 20-25 cm.
5. The method for preparing the intermediate layer of the lithium-sulfur battery comprising the metal selenide-supported carbon nanofibers according to claim 1, wherein the nanofiber film prepared in the step S1 is heated to 250-300 ℃ at a heating rate of 2-5 ℃/min in an air atmosphere, and is subjected to pre-oxidation while being kept warm; and after cooling, heating the nanofiber membrane to 500-700 ℃ at a heating rate of 5-10 ℃/min in a nitrogen atmosphere, preserving heat, carbonizing and selenizing to obtain the metal selenide loaded carbon nanofiber membrane, and cutting the carbon nanofiber membrane by using a slicer to obtain the intermediate layer material of the lithium-sulfur battery.
6. The lithium-sulfur battery is characterized by comprising a positive electrode, an intermediate layer, a diaphragm and a negative electrode, wherein the positive electrode, the intermediate layer, the diaphragm and the negative electrode are sequentially assembled in an argon atmosphere, and an electrolyte is added; the intermediate layer employs the metal selenide-supported carbon nanofiber intermediate layer prepared by the method of claim 1.
7. The lithium sulfur battery according to claim 6, wherein the method for preparing the positive electrode material comprises: the CMK-3 and the sulfur powder with the mass ratio of 3:7 are subjected to heat preservation for 12 hours at the temperature of 155 ℃ by a melting method to prepare a sulfur composite material; preparing a sulfur composite material into slurry containing a conductive agent, a bonding agent and an organic solvent; coating the slurry on an aluminum foil current collector to serve as a positive pole piece of the lithium-sulfur battery, wherein the surface loading capacity is 1mg/cm2。
8. The lithium sulfur battery as defined in claim 6 wherein the mass ratio of the sulfur composite, the conductive agent and the binder is 7: 2: 1.
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| CN113346084A (en) * | 2021-05-31 | 2021-09-03 | 华中科技大学 | Conductive catalytic composite material interlayer for battery, and preparation method and application thereof |
| CN113823791A (en) * | 2021-09-14 | 2021-12-21 | 西安交通大学 | Lithium-sulfur battery positive electrode barrier layer material and preparation method thereof |
| CN114267818A (en) * | 2021-12-24 | 2022-04-01 | 淮北师范大学 | Preparation method and application of positive electrode polysulfide buffer layer for improving cycle performance of lithium-sulfur battery |
| CN114512658A (en) * | 2022-02-28 | 2022-05-17 | 新锦彦(广东)新能源有限公司 | FeTiO3-TiO2Porous carbon nanofiber membrane material loaded by heterostructure and application of porous carbon nanofiber membrane material in sodium-selenium battery |
| CN114725333A (en) * | 2022-03-08 | 2022-07-08 | 华中科技大学 | Lithium-sulfur battery composite positive electrode material, and preparation and application thereof |
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| CN115036504A (en) * | 2022-07-22 | 2022-09-09 | 济南易航新材料科技有限公司 | Flower-like vanadium diselenide @ carbon fiber nano material, preparation method and application thereof, and magnesium-lithium double-ion battery |
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