CN113130879B - Preparation method of high-adsorption catalytic performance cathode material of lithium-sulfur battery - Google Patents
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Abstract
The invention belongs to the technical field of lithium-sulfur batteries, and particularly relates to a preparation method of a high-adsorption catalytic performance cathode material of a lithium-sulfur battery. The preparation method of the cathode material with high adsorption and catalytic performance for the lithium-sulfur battery comprises the following steps: (1) preparing a silicon dioxide ball dispersion liquid: adopting a sol-gel method; (2) preparing a highly uniform phenolic resin ethanol solution: adopting an aldehyde phenol addition reaction; (3) preparation of SiO2a/AAO dual template; (4) preparing Ta/CNW; (5) preparation S @ Ta/CNW.
Description
Technical Field
The invention belongs to the technical field of lithium-sulfur batteries, and particularly relates to a preparation method of a high-adsorption catalytic performance cathode material of a lithium-sulfur battery.
Background
With the rapid development of society and the increase of population in the world, the increasing exhaustion of fossil fuels and the huge environmental problems brought by the traditional fossil energy, people have urgent needs for energy and new energy for sustainable development. Renewable energy sources such as nuclear energy, wind energy, solar energy and the like in new energy industry are continuously developed at a high speed, and the new energy industry generally faces the characteristics of seasonality, periodicity and the like, and always needs to be stored and redistributed first, so the development of energy storage equipment directly restricts the development speed of the new energy industry. To address the challenges of energy crisis and environmental pollution, it is currently a critical task to develop environmentally friendly and high performance energy storage and conversion systems.
Although the development of lithium ion batteries has matured sufficiently, their specific energy has been very close to the theoretical specific energy (300 mAh. g) of their corresponding materials-1) But still can not meet the increasing demands of people on novel batteries with environmental protection and high specific energy, and the problem that the next generation of lithium secondary battery cathode material with high energy density, environmental protection and low cost is urgently needed to be solved is searched. Lithium sulfur battery with metallic Li as negative electrode and elemental sulfur as active positive electrode exhibited a freshness of 2600Wh kg-1Theoretical energy density and high specific discharge capacity of (1675 mAh. g-1) And sulfur is non-toxic and low-cost and friendly, so the system has become one of the secondary batteries with the most potential and wide application in the next generation.
The working mechanism of lithium-sulfur batteries differs from that of "intercalation/deintercalation" type lithium-ion batteries, which rely mainly on S8And Li perform a series of reversible electrochemical reactions to complete the charge/discharge process to provide energy. Although the lithium-sulfur battery has the advantages of high specific capacity and energy density, environmental friendliness, rich sulfur resources and the like, the problems of low actual discharge capacity, poor cycle stability, serious self-discharge, reduced safety and the like of the battery exist due to the physical and chemical characteristics of the active material and the discharge product, and the commercial production of the lithium-sulfur battery is severely restricted.
Therefore, lithium sulfur batteries, if widely used, must address several key challenges: (1) sulphur and end product Li2S2/Li2S has low conductivity. The conductivity of the active substance sulfur at room temperature is only 5 x 10-30S﹒cm-1The insulating property greatly increases the internal resistance of the battery, and reduces the utilization rate and rate capability of the active material. (2) The shuttle effect of polysulphides. Long-chain polysulfide intermediate Li generated by positive electrode in discharge reaction process2Sx(x is more than or equal to 4 and less than or equal to 8) is easy to dissolve in the common ether electrolyte, can penetrate through a diaphragm and migrate and diffuse to a negative electrode under the action of concentration gradient force, and then part of Li2SnFormation of insoluble short-chain polysulphides Li in combination with lithium metal anodes2S2/Li2And S, the surface of the negative electrode is corroded and passivated, and the further reaction is hindered, so that the coulomb efficiency of the battery is reduced. Under the drive of electric field force during charging, short-chain polysulfide on the lithium negative electrode returns to the sulfur positive electrode and is oxidized again into long-chain polysulfide in the charging process; causing fatal problems of rapid capacity decay, reduced coulombic efficiency, severe self-discharge, shortened cycle life and the like of the lithium-sulfur battery. (3) The volume expands. Density of Quadrature-phase Cyclic elemental Sulfur (2.03 g. cm-3) Proportional powerElectric end product Li2S(1.66g﹒cm-3) Much larger, resulting in a large volume change (about 80%) during charging and discharging of the lithium-sulfur battery. Resulting in pulverization of the electrode structure, separation of the active material from the conductive additive, current collector, and leakage of soluble polysulfide from the positive electrode.
In order to solve the problems of the lithium-sulfur battery, researchers propose various strategies to modify the lithium-sulfur battery system in an all-round manner, including designing a novel positive electrode material, developing a novel electrolyte, modifying a diaphragm, protecting a lithium negative electrode and the like. In the prior art, activated carbon, ordered mesoporous carbon, multi-walled carbon nanotubes, graphene and the like are compounded with sulfur to form a sulfur/carbon composite material, and on one hand, the carbon material serving as a conductive carrier can improve the conductivity of a sulfur anode; on the other hand, sulfur is embedded into the pore canal and pores of the carbon material, so that the polysulfide intermediate product can be prevented from being dissolved in the electrolyte to a certain extent, and the cycle performance is improved. However, the nonpolar carbon material interacts only weakly physically with the polar polysulfides and is not sufficient to completely improve the shuttling effect of the polysulfides.
Disclosure of Invention
The invention aims to provide a preparation method of a cathode material with high adsorption and catalysis performance for a lithium-sulfur battery, aiming at the defects, and the cathode material obtained by the preparation method can obviously improve the adsorption and catalysis effect on lithium polysulfide and the specific capacity of the battery.
The technical scheme of the invention is as follows: a preparation method of a high-adsorption catalytic performance cathode material of a lithium-sulfur battery comprises the following steps:
(1) preparing a silicon dioxide ball dispersion liquid: adopting a sol-gel method;
(2) preparing a highly uniform phenolic resin ethanol solution: adopting an aldehyde phenol addition reaction;
(3) preparation of SiO2AAO double templates: placing the AAO template in the silicon dioxide ball dispersion liquid obtained in the step (1), standing, and naturally volatilizing to obtain SiO2a/AAO dual template;
(4) preparing Ta/CNW: ultrasonically treating tantalum ethoxide, phenolic resin and absolute ethyl alcohol to form a mixed solution, and then treating the SiO obtained in the step (3)2Placing the AAO double-template in the mixed solution, standing, placing in an oven for curing, transferring to a tubular furnace, heating to 800-1000 ℃ at a heating rate of 2-8 ℃/min under Ar gas atmosphere, and preserving heat for 2-4 hours for high-temperature carbonization; naturally cooling to room temperature after the reaction is finished, collecting a product, removing the template by using 5% HF, and washing to be neutral by using deionized water to obtain the tantalum monoatomic-doped carbon nanowire Ta/CNW; the obtained Ta/CNW is formed by doping tantalum monoatomic atoms dispersed at the atomic level on mesoporous carbon nanowires; the nano-wire has a uniform and ordered spherical mesoporous structure, and the wall of the hole of the nano-wire is provided with highly dispersed Ta monatomic;
(5) preparation S @ Ta/CNW: firstly, weighing nano sulfur powder and Ta/CNW obtained in the step (4) to be mixed and ground; and then transferring the ground powder into a reaction kettle, and preserving heat for 12 hours at 100-200 ℃ to obtain S @ Ta/CNW.
1 AAO template in the step (3); the volume of the silica sphere dispersion was 5 mL. And (4) standing for 4 days in the step (3).
In the step (4), 50-200 mu L of tantalum ethoxide, 200-800 mu L of phenolic resin and 1-3 mL of absolute ethyl alcohol are used.
And (4) standing for 1-3 days, wherein the curing temperature is 50-150 ℃, and the curing time is 12-48 hours.
In the step (5), the nano sulfur powder is prepared by the following steps in percentage by mass: Ta/CNW was 3: 1.
The invention has the beneficial effects that: in the preparation method, in the chemical reaction process for preparing the carbon nano wire, Anodic Aluminum Oxide (AAO) and silicon dioxide are used as double templates, phenolic resin is used as a carbon source, and the most important point is that the adding proportion of ethanol and tantalum is strictly controlled in the reaction process so as to limit the formation of other tantalum compounds, so that the tantalum monoatomic substance dispersed in an atomic level is doped on the carbon nano wire (Ta/CNW) rich in mesopores.
Tantalum monoatomic atoms dispersed at atomic level are doped into the carbon nano-wires containing abundant mesopores to adjust the electronic structure of the carbon atoms, so that polysulfide on the adsorption/catalysis surface is activated. The prepared positive electrode material not only contains abundant mesopores to further increase the specific surface area, and is beneficial to the storage of active substances, so that the positive electrode has good conductivity and can relieve the problem of volume expansion in the charging and discharging process; and the synthesis of the tantalum monoatomic can realize the maximum utilization rate of active metal atoms, strong coordination between the metal atoms and a base and unique electronic effect, can obviously improve the adsorption catalysis of the material on lithium polysulfide, and further improves the specific capacity of the battery, the integral conductivity of the electrode and the rate capability of the lithium-sulfur battery.
Drawings
FIG. 1 is a scanned image of Ta/CNW as described in example 1.
FIG. 2 is a transmission image of Ta/CNW as described in example 1.
FIG. 3 is a high angle annular dark field image-scanning transmission electron microscope of Ta/CNW as described in example 1.
FIG. 4 is a graph comparing the voltage-specific capacity curves of S @ Ta/CNW as a cathode material for lithium sulfur batteries as described in examples 1-3.
Detailed Description
The present invention will be described in detail with reference to examples.
Example 1
The preparation method of the cathode material with high adsorption and catalytic performance for the lithium-sulfur battery comprises the following steps:
(1) preparing a silicon dioxide ball dispersion liquid: adopting a sol-gel method: adding tetraethoxysilane into a mixed solution of a catalyst and an alcohol solvent, and reacting to prepare a nano silicon dioxide ball;
(2) preparing a highly uniform phenolic resin ethanol solution: adopting an aldehyde phenol addition reaction: synthesized by phenol, formaldehyde and sodium hydroxide;
(3) preparation of SiO2AAO double templates: placing 1 piece of AAO template in 5mL of silicon dioxide ball dispersion liquid obtained in the step (1), standing for 4 days, and naturally volatilizing to obtain SiO2a/AAO dual template;
(4) preparing Ta/CNW: firstly, ultrasonically treating 100 mu L of tantalum ethoxide, 500 mu L of phenolic resin and 2mL of absolute ethyl alcohol to form a mixed solution, and then treating the SiO obtained in the step (3)2Placing the AAO double-template in the mixed solution, standing for 2 days, placing in an oven, and placing in a vacuum oven at 1Curing at 00 ℃ for 24 hours, transferring the mixture into a tubular furnace, heating the mixture to 900 ℃ at the heating rate of 5 ℃/min under the Ar atmosphere, and preserving the heat for 3 hours to carry out high-temperature carbonization; naturally cooling to room temperature after the reaction is finished, collecting a product, removing the template by using 5% HF, and washing to be neutral by using deionized water to obtain the tantalum monoatomic-doped carbon nanowire Ta/CNW; the obtained Ta/CNW is formed by doping tantalum monoatomic atoms dispersed at the atomic level on mesoporous carbon nanowires; the nano-wire has a uniform and ordered spherical mesoporous structure, and the wall of the hole of the nano-wire is provided with highly dispersed Ta monatomic;
(5) preparation S @ Ta/CNW: firstly, nano sulfur powder according to mass ratio: weighing nano sulfur powder according to the proportion of Ta/CNW of 3:1 and mixing and grinding the nano sulfur powder and the Ta/CNW obtained in the step (4); and then transferring the ground powder into a reaction kettle, and preserving heat at 155 ℃ for 12 hours to obtain S @ Ta/CNW.
As is evident from FIG. 1, the average diameter of the prepared nanowires is about 340nm, the nanowires are rich in uniform and ordered spherical mesopores, and the pore diameter is about 40 nm.
As is apparent from fig. 2, the ordered mesoporous structure on the nanowires.
As is evident from fig. 3, there are highly dispersed Ta monoatomic atoms on the nanowire pore walls, with no significant particle aggregation, demonstrating successful loading of atomic-scale Ta onto the carbon matrix.
Example 2
The preparation method of the cathode material with high adsorption and catalytic performance for the lithium-sulfur battery comprises the following steps:
(1) preparing a silicon dioxide ball dispersion liquid: adopting a sol-gel method: adding tetraethoxysilane into a mixed solution of a catalyst and an alcohol solvent, and reacting to prepare a nano silicon dioxide ball;
(2) preparing a highly uniform phenolic resin ethanol solution: adopting an aldehyde phenol addition reaction: synthesized by phenol, formaldehyde and sodium hydroxide;
(3) preparation of SiO2AAO double templates: placing 1 piece of AAO template in 5mL of silicon dioxide ball dispersion liquid obtained in the step (1), standing for 4 days, and naturally volatilizing to obtain SiO2a/AAO dual template;
(4) preparing Ta/CNW: firstly 50 mu L of ethanolUltrasonically treating tantalum, 200 mu L of phenolic resin and 1mL of absolute ethyl alcohol to form a mixed solution, and then treating the SiO obtained in the step (3)2Placing the AAO double-template in the mixed solution, standing for 1 day, placing in an oven, curing at 80 ℃ for 12 hours, transferring to a tubular furnace, heating to 800 ℃ at a heating rate of 2 ℃/min under Ar gas atmosphere, and preserving heat for 2 hours to carry out high-temperature carbonization; naturally cooling to room temperature after the reaction is finished, collecting a product, removing the template by using 5% HF, and washing to be neutral by using deionized water to obtain the tantalum monoatomic-doped carbon nanowire Ta/CNW; the obtained Ta/CNW is formed by doping tantalum monoatomic atoms dispersed at the atomic level on mesoporous carbon nanowires; the nano-wire has a uniform and ordered spherical mesoporous structure, and the wall of the hole of the nano-wire is provided with highly dispersed Ta monatomic;
(5) preparation S @ Ta/CNW: firstly, nano sulfur powder according to mass ratio: weighing nano sulfur powder according to the proportion of Ta/CNW of 3:1 and mixing and grinding the nano sulfur powder and the Ta/CNW obtained in the step (4); and then transferring the ground powder into a reaction kettle, and preserving heat for 12 hours at 100 ℃ to obtain S @ Ta/CNW.
Example 3
The preparation method of the cathode material with high adsorption and catalytic performance for the lithium-sulfur battery comprises the following steps:
(1) preparing a silicon dioxide ball dispersion liquid: adopting a sol-gel method: adding tetraethoxysilane into a mixed solution of a catalyst and an alcohol solvent, and reacting to prepare a nano silicon dioxide ball;
(2) preparing a highly uniform phenolic resin ethanol solution: adopting an aldehyde phenol addition reaction: synthesized by phenol, formaldehyde and sodium hydroxide;
(3) preparation of SiO2AAO double templates: placing 1 piece of AAO template in 5mL of silicon dioxide ball dispersion liquid obtained in the step (1), standing for 4 days, and naturally volatilizing to obtain SiO2a/AAO dual template;
(4) preparing Ta/CNW: firstly, ultrasonically treating 200 mu L of tantalum ethoxide, 800 mu L of phenolic resin and 3mL of absolute ethyl alcohol to form a mixed solution, and then treating the SiO obtained in the step (3)2Placing the AAO double-template in the mixed solution, standing for 3 days, placing in an oven, curing at 150 ℃ for 48 hours, and transferring to a tubular furnace under Ar atmosphere at the temperature rise of 8 ℃/minRaising the temperature to 1000 ℃ at a speed, and preserving the heat for 4 hours to carry out high-temperature carbonization; naturally cooling to room temperature after the reaction is finished, collecting a product, removing the template by using 5% HF, and washing to be neutral by using deionized water to obtain the tantalum monoatomic-doped carbon nanowire Ta/CNW; the obtained Ta/CNW is formed by doping tantalum monoatomic atoms dispersed at the atomic level on mesoporous carbon nanowires; the nano-wire has a uniform and ordered spherical mesoporous structure, and the wall of the hole of the nano-wire is provided with highly dispersed Ta monatomic;
(5) preparation S @ Ta/CNW: firstly, nano sulfur powder according to mass ratio: weighing nano sulfur powder according to the proportion of Ta/CNW of 3:1 and mixing and grinding the nano sulfur powder and the Ta/CNW obtained in the step (4); and then transferring the ground powder into a reaction kettle, and preserving heat for 12 hours at 200 ℃ to obtain S @ Ta/CNW.
As is apparent from fig. 4, example 1 has a higher actual specific discharge capacity and smaller polarization than those of examples 2 and 3.
Claims (4)
1. A preparation method of a high-adsorption catalytic performance cathode material of a lithium-sulfur battery is characterized by comprising the following steps:
(1) preparing a silicon dioxide ball dispersion liquid: adopting a sol-gel method;
(2) preparing a highly uniform phenolic resin ethanol solution: adopting an aldehyde phenol addition reaction;
(3) preparation of SiO2AAO double templates: placing the AAO template in the silicon dioxide ball dispersion liquid obtained in the step (1), standing, and naturally volatilizing to obtain SiO2a/AAO dual template;
(4) preparing Ta/CNW: ultrasonically treating tantalum ethoxide, phenolic resin and absolute ethyl alcohol to form a mixed solution, wherein the tantalum ethoxide is 50-200 mu L, the phenolic resin is 200-800 mu L, and the absolute ethyl alcohol is 1-3 mL; then, the SiO obtained in the step (3) is put into2 Placing the AAO double-template in the mixed solution, standing, placing in an oven for curing, transferring to a tubular furnace, heating to 800-1000 ℃ at a heating rate of 2-8 ℃/min under Ar gas atmosphere, and preserving heat for 2-4 hours for high-temperature carbonization; naturally cooling to room temperature after the reaction is finished, collecting a product, removing the template by adopting 5 percent HF, and washing the product to be neutral by using deionized water to obtain the tantalum monoatomic atomDoped carbon nanowires Ta/CNW; the obtained Ta/CNW is formed by doping tantalum monoatomic atoms dispersed at the atomic level on mesoporous carbon nanowires; the nano-wire has a uniform and ordered spherical mesoporous structure, and the wall of the hole of the nano-wire is provided with highly dispersed Ta monatomic;
(5) preparation S @ Ta/CNW: firstly, weighing nano sulfur powder and Ta/CNW obtained in the step (4) to be mixed and ground; and then transferring the ground powder into a reaction kettle, and preserving heat for 12 hours at 100-200 ℃ to obtain S @ Ta/CNW.
2. The preparation method of the cathode material with high adsorption and catalytic performance for the lithium-sulfur battery according to claim 1, wherein the AAO template in the step (3) is 1 piece; the amount of the silica sphere dispersion was 5mL, and the standing time in the step (3) was 4 days.
3. The preparation method of the cathode material with high adsorption and catalytic performance for the lithium-sulfur battery according to claim 1, wherein the standing time in the step (4) is 1-3 days, the curing temperature is 50-150 ℃, and the curing time is 12-48 hours.
4. The preparation method of the cathode material with high adsorption and catalytic performance for the lithium-sulfur battery as claimed in claim 1, wherein the mass ratio of the nano-sulfur powder in the step (5): Ta/CNW was 3: 1.
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