CN111403698A - Novel efficient lithium-sulfur battery positive electrode material and preparation method thereof - Google Patents
Novel efficient lithium-sulfur battery positive electrode material and preparation method thereof Download PDFInfo
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Abstract
The invention belongs to the technical field of lithium-sulfur batteries, and particularly relates to a novel efficient lithium-sulfur battery positive electrode material and a preparation method thereof. The anode material is S @ Nb2C/Nb2O5A composite material. The positive electrode material improves the utilization rate of active substances, and further improves the electrochemical performance and the cycling stability of the lithium-sulfur battery.
Description
Technical Field
The invention belongs to the technical field of lithium-sulfur batteries, and particularly relates to a novel efficient lithium-sulfur battery positive electrode material and a preparation method thereof.
Background
As the depletion of fossil fuels and their environmental impact have become increasingly of concern, the demand for energy storage systems has also increased rapidly. Among the existing energy storage technologies, lithium ion batteries are considered to be the most widely used battery type at present due to their high energy density and long cycle life. However, even though the specific capacity of the lithium ion battery is close to the theoretical specific capacity of 300mAh & g at present-1But still can not satisfy the requirements of human production and birthWith the increasing energy demand, especially with the popularization of portable electronic devices, mobile power sources and new energy automobiles, the relatively low energy density of lithium ion batteries is increasingly unable to meet the demand of large energy storage devices, and therefore, it is one of the hot spots of recent research to find an energy storage material with higher energy density, lighter weight, smaller volume and longer cycle life. In recent years, the lithium sulfur battery using elemental sulfur as the battery anode and metal lithium as the cathode material has attracted the attention of researchers at home and abroad, and the elemental sulfur has 1675 mAh.g-1Although the lithium-sulfur battery has a plurality of advantages, the lithium-sulfur battery still has some defects that (1) the elemental sulfur and the discharge product L i thereof2S2And L i2The conductivity of S is poor; (2) due to the density change of the substance in the reaction process, the volume expansion effect is caused; (3) the shuttling effect is due to the dissolution of lithium polysulphides. The improvement of the specific capacity, the cycle life, the cycle stability and other performances of the existing lithium-sulfur battery is seriously limited by the problems, and the development of a novel lithium-sulfur battery anode material and the improvement of the utilization rate of active substances in an electrode material are of great importance to solve the problems related to each other.
Aiming at the problems of the lithium-sulfur battery, the modified material of the sulfur anode needs to have the following advantages: (1) good conductivity, which is beneficial to the transmission of electrons in the electrode and promotes the reaction kinetics of a solid/liquid interface; (2) the composite material has a pore structure with proper and rich size and certain mechanical strength, can highly disperse active substance sulfur on a matrix material, and an internal pore network can ensure the transmission of ions and electrons, relieve volume expansion and shrinkage stress in the discharging process and avoid structural collapse; (3) the lithium polysulfide is adsorbed by proper strength, so that the purposes of inhibiting shuttle effect, improving the utilization rate of active substances and improving the long-range stability of the battery are achieved; (4) has certain catalytic action on the conversion reaction between sulfur species in the lithium-sulfur battery.
Disclosure of Invention
The invention aims to provide a novel and efficient lithium-sulfur battery positive electrode material and a preparation method thereof, aiming at the defects, the positive electrode material improves the utilization rate of active substances, and further improves the electrochemical performance and the cycling stability of the lithium-sulfur battery.
The technical scheme of the invention is as follows: a novel and efficient positive electrode material S @ Nb for lithium-sulfur battery2C/Nb2O5A composite material.
The S @ Nb2C/Nb2O5Nb in composite material2C/Nb2O5Is an accordion-shaped multilayer structure.
The S @ Nb is adopted in the preparation method of the novel high-efficiency lithium-sulfur battery positive electrode material2C/Nb2O5Nb in composite material2C/Nb2O5Prepared by a water vapor etching method.
The preparation method of the novel high-efficiency lithium-sulfur battery positive electrode material comprises the following steps:
(1)Nb2c, preparation: mixing Nb with2Mixing AlC powder and HF water solution, stirring to obtain Nb2C；
(2)Nb2C/Nb2O5The preparation of (1): taking Nb obtained in the step (1)2C, carrying out water vapor etching to prepare Nb2C/Nb2O5；
(3)S@Nb2C/Nb2O5Preparing a composite material: firstly, the prepared Nb is2C/Nb2O5Mixing with nanometer sulfur, and grinding; then dropwise adding carbon disulfide, grinding again, and then putting into a reaction kettle for hydrothermal reaction to obtain S @ Nb2C/Nb2O5A composite material.
Nb in the step (1)20.02-0.1 g AlC powder and 10-50 m L HF aqueous solution.
Nb in the step (1)2The AlC powder is 200-400 meshes; the mass fraction of the HF aqueous solution is 40-50%.
The stirring in the step (1) is specifically as follows: stirring for 22-72 h at 45-60 ℃.
Nb obtained in the step (2)2C is 0.01 to 0.08 g.
The steam etching in the step (2) specifically comprises the following steps: taking Nb2C, placing the porcelain boat in a tube furnace, installing a water vapor etching device, raising the temperature to 500-600 ℃ at the temperature rise rate of 1-10 ℃/min, and preserving the heat at the temperature for 5-30 min to obtain Nb2C/Nb2O5。
The step (3) is specifically as follows: firstly, weighing nano sulfur and prepared Nb2C/Nb2O5Mixing to obtain a mixture, wherein the mass ratio of nano sulfur: nb2C/Nb2O51-3: 1; placing the mixture in a mortar and grinding the mixture into uniform and fine powder; then dropwise adding carbon disulfide into the mixture powder in the mortar, fully grinding again, putting into a reaction kettle, and carrying out hydrothermal reaction at 155 ℃ for 12-24 h to obtain S @ Nb2C/Nb2O5A composite material.
The invention has the beneficial effects that: the novel efficient lithium-sulfur battery positive electrode material is S @ Nb2C/Nb2O5Composite material of Nb2C/Nb2O5Is an accordion-shaped multilayer structure.
Morphologically speaking, Nb with accordion-like multilayer structure2C/Nb2O5As a sulfur carrier, can better coat sulfur and reduce volume expansion of sulfur during circulation, and Nb2C/Nb2O5The layered structure of the material exposes more active sites, accelerates the transmission efficiency of electrons and ions, improves the mass transfer rate, promotes the redox reaction in the charging and discharging process of the lithium-sulfur battery, and can promote the transformation of polysulfide, so that the utilization rate of active substances can be improved, thereby improving the electrochemical performance and the cycling stability of the lithium-sulfur battery.
From a matter standpoint, Nb2O5As transition group metal oxides, adsorptivity can be increased, i.e., polysulfide is adsorbed better and more, thereby inhibiting the shuttling effect of polysulfide; nb2C as MXene can increase its conductivity in a lithium sulfur battery.
Meanwhile, the invention fully considers the structural problem of the sulfur-based composite material in the lithium-sulfur battery anode material and innovatively provides the method for preparing Nb by using the water vapor etching method2C/Nb2O5The process of (1). Compared with other methods, the water vapor etching method is safer, and the water vapor etching can form small holes of about 10nm on the surface and inside of the substance. The adopted water vapor etching method is easy and effective, is easy to realize large-scale preparation and low-cost industrialization of the cathode material, and has high yield and industrial feasibility.
Drawings
FIG. 1 shows Nb prepared in example 12XRD pattern of C.
FIG. 2 shows Nb prepared in example 12SEM image of C.
FIG. 3 shows Nb prepared in example 12C/Nb2O5XRD pattern of (a).
FIG. 4 shows Nb prepared in example 12C/Nb2O5SEM image of (d).
FIG. 5 is the S @ Nb prepared in example 12C/Nb2O5The composite material is used as a lithium-sulfur battery cathode material for an electrochemical charge-discharge curve of a lithium-sulfur battery.
Detailed Description
The related raw materials are all obtained by commercial purchase, and the specific commercial manufacturer is Beijing Beike New materials science and technology company.
Example 1
The novel efficient lithium-sulfur battery positive electrode material is S @ Nb2C/Nb2O5A composite material. Nb in the composite material2C/Nb2O5Is an accordion-shaped multilayer structure.
The preparation method of the novel high-efficiency lithium-sulfur battery positive electrode material comprises the following steps:
(1)Nb2c, preparation: firstly, 0.1g of 200 mesh Nb2Mixing AlC powder with HF aqueous solution with the mass fraction of 50m L being 40%, and then stirring for 22h at 45 ℃ to obtain Nb2C；
(2)Nb2C/Nb2O5The preparation of (1): taking 0.05g of Nb obtained in the step (1)2C, placing the porcelain boat in a tube furnace, installing a water vapor etching device, raising the temperature to 600 ℃ at the heating rate of 10 ℃/min, and preserving the heat for 5min at the temperature to obtain Nb2C/Nb2O5；
(3)S@Nb2C/Nb2O5Preparing a composite material: firstly, weighing nano sulfur and prepared Nb2C/Nb2O5Mixing to obtain a mixture, wherein the mass ratio of nano sulfur: nb2C/Nb2O5Is 3: 1; placing the mixture in a mortar and grinding the mixture into uniform and fine powder; then dropwise adding carbon disulfide into the mixture powder in the mortar, fully grinding again, putting into a reaction kettle, and keeping the temperature for 12 hours at 155 ℃ to perform hydrothermal reaction to obtain S @ Nb2C/Nb2O5A composite material.
As can be seen from FIG. 1, Nb is predominant2C substance, and unavoidable AlF3Impurities.
As can be seen from FIG. 2, Nb2C is an accordion multilayer structure.
As can be seen from FIG. 3, Nb2C/Nb2O5In the presence of Nb2C and Nb2O5Two kinds of substances.
As can be seen from FIG. 4, Nb2C/Nb2O5Maintaining the accordion-like multilayer structure.
As can be seen from FIG. 5, the first discharge capacity of the material obtained in this example as a positive electrode material for a lithium-sulfur battery was as high as 1057.3mAh g at a current density of 0.2C-1。
Example 2
The preparation method of the novel high-efficiency lithium-sulfur battery positive electrode material comprises the following steps:
(1)Nb2c, preparation: firstly, 0.02g of 200 mesh Nb2Mixing AlC powder with 10m of HF aqueous solution with the mass fraction of L being 50%, and then stirring for 22h at 60 ℃ to obtain Nb2C；
(2)Nb2C/Nb2O5The preparation of (1): taking 0.01g of Nb obtained in the step (1)2C, placing the porcelain boat in a tube furnace, installing a water vapor etching device, raising the temperature to 500 ℃ at the rate of 1 ℃/min, and preserving the heat for 5min at the temperature to obtain Nb2C/Nb2O5；
(3)S@Nb2C/Nb2O5Preparing a composite material: firstly, weighing nano sulfur and prepared Nb2C/Nb2O5Mixing to obtain a mixture, wherein the mass ratio of nano sulfur: nb2C/Nb2O5Is 1: 1; placing the mixture in a mortar and grinding the mixture into uniform and fine powder; then dropwise adding carbon disulfide into the mixture powder in the mortar, fully grinding again, putting into a reaction kettle, and keeping the temperature for 12 hours at 155 ℃ to perform hydrothermal reaction to obtain S @ Nb2C/Nb2O5A composite material.
Claims (10)
1. A novel high-efficiency positive electrode material of a lithium-sulfur battery is characterized in that the positive electrode material is S @ Nb2C/Nb2O5A composite material.
2. The novel high-efficiency positive electrode material for lithium-sulfur batteries according to claim 1, wherein S @ Nb is2C/Nb2O5Nb in composite material2C/Nb2O5Is an accordion-shaped multilayer structure.
3. The preparation method of the novel high-efficiency lithium-sulfur battery positive electrode material as claimed in claim 1, wherein S @ Nb is2C/Nb2O5Nb in composite material2C/Nb2O5Prepared by a water vapor etching method.
4. The preparation method of the novel high-efficiency lithium-sulfur battery positive electrode material according to claim 3, comprising the following steps:
(1)Nb2c, preparation: mixing Nb with2Mixing AlC powder and HF water solution and stirring to prepareObtaining Nb2C；
(2)Nb2C/Nb2O5The preparation of (1): taking Nb obtained in the step (1)2C, carrying out water vapor etching to prepare Nb2C/Nb2O5；
(3)S@Nb2C/Nb2O5Preparing a composite material: firstly, the prepared Nb is2C/Nb2O5Mixing with nanometer sulfur, and grinding; then dropwise adding carbon disulfide, grinding again, and then putting into a reaction kettle for hydrothermal reaction to obtain S @ Nb2C/Nb2O5A composite material.
5. The method for preparing the novel high-efficiency lithium-sulfur battery cathode material as claimed in claim 4, wherein Nb is adopted in the step (1)20.02-0.1 g AlC powder and 10-50 m L HF aqueous solution.
6. The method for preparing the novel high-efficiency lithium-sulfur battery cathode material as claimed in claim 5, wherein Nb is adopted in the step (1)2The AlC powder is 200-400 meshes; the mass fraction of the HF aqueous solution is 40-50%.
7. The preparation method of the novel high-efficiency lithium-sulfur battery cathode material according to claim 4, wherein the stirring in the step (1) is specifically as follows: stirring for 22-72 h at 45-60 ℃.
8. The method for preparing the novel high-efficiency positive electrode material of the lithium-sulfur battery as claimed in claim 5, wherein the Nb obtained in the step (2)2C is 0.01 to 0.08 g.
9. The preparation method of the novel high-efficiency lithium-sulfur battery cathode material according to claim 4, wherein the steam etching in the step (2) is specifically as follows: taking Nb2C, placing the porcelain boat in a tube furnace, installing a water vapor etching device, raising the temperature to 500-600 ℃ at a heating rate of 1-10 ℃/min, and raising the temperature at the temperaturePreserving heat for 5-30 min to obtain Nb2C/Nb2O5。
10. The preparation method of the novel high-efficiency lithium-sulfur battery cathode material according to claim 4, wherein the step (3) is specifically as follows: firstly, weighing nano sulfur and prepared Nb2C/Nb2O5Mixing to obtain a mixture, wherein the mass ratio of nano sulfur: nb2C/Nb2O51-3: 1; placing the mixture in a mortar and grinding the mixture into uniform and fine powder; then dropwise adding carbon disulfide into the mixture powder in the mortar, fully grinding again, putting into a reaction kettle, and carrying out hydrothermal reaction at 155 ℃ for 12-24 h to obtain S @ Nb2C/Nb2O5A composite material.
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