CN108390060B - Nano petal-shaped nickel-cobalt-molybdenum ternary metal sulfide and preparation method and application thereof - Google Patents
Nano petal-shaped nickel-cobalt-molybdenum ternary metal sulfide and preparation method and application thereof Download PDFInfo
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Abstract
The invention discloses a nanometer petal-shaped nickel-cobalt-molybdenum ternary metal sulfide, a preparation method and an application thereof, wherein the preparation method comprises the following steps: dissolving ammonium molybdate tetrahydrate, nickel nitrate hexahydrate and cobalt nitrate hexahydrate in deionized water, and after completely dissolving uniformly, adding sulfur powder and completely dispersing to form a uniform colloidal solution; adding hydrazine hydrate into the colloidal solution, fully stirring, and then transferring into an oven for solvothermal reaction; and (3) sequentially washing the product of the solvothermal reaction with alcohol and water alternately, drying, and then transferring to a high-temperature tubular furnace for high-temperature treatment to finally obtain the nano petal-shaped ternary metal sulfide material. The invention greatly improves the capacity of the metal material by regulating the shape of the material and the doping process of the sulfur element, solves the problems of excessive side reaction, unstable structure and poor conductivity of elemental sulfur as the lithium ion battery anode material, and is expected to greatly improve the energy density of the material.
Description
Technical Field
The invention relates to the field of lithium ion battery anode materials, in particular to a nanometer petal-shaped nickel-cobalt-molybdenum ternary metal sulfide and a preparation method and application thereof.
Background
In recent years, in order to cope with the increasingly serious problems of energy depletion and environmental pollution and greenhouse effect caused thereby, research on novel energy sources and conversion methods is actively conducted in various countries, and among them, research on lithium ion batteries, such as mobile power sources, Electric Vehicles (EVs), and the like, is receiving attention. At present, the bottlenecks restricting the large-scale development of the lithium ion battery are mainly three: the first is the cost of the lithium battery, the manufacturing cost of the current lithium ion battery pack is about $ 900-1000/kWh, which is much higher than $ 300/kWh required by commercialization, and needs to be greatly reduced; secondly, the cycle life and the shelf life of the lithium battery are prolonged, the performance of the battery is reduced, and the replacement requirement of the lithium battery is increased; and thirdly, the safety of the lithium battery. However, the key for determining the cost and the performance of the lithium ion power battery is the material, and the material of the lithium ion power battery determines the development route and the operation mode of the electric automobile. Therefore, the bottleneck problem of the lithium ion power battery is broken through, and the key point is the solution of the material problem.
The lithium ion battery commercialized at present is mainlyBy using LiCoO2And LiFeO2As a positive electrode material, however, there are problems such as high production cost, low capacity and poor safety. LiNixCoyMnzO2The ternary cathode material has the characteristics of good cycle performance, high safety, low cost and the like, so that the ternary cathode material becomes the most concerned lithium ion battery cathode material in recent years. The ternary metal sulfide can improve the capacity of the whole material by introducing a proper amount of sulfur element, so that the energy density of the battery can be greatly improved, the manufacturing cost of the battery is reduced, and the ternary metal sulfide has obvious application value.
Disclosure of Invention
Based on the technical problems in the background art, the invention provides a nanometer petal-shaped nickel-cobalt-molybdenum ternary metal sulfide and a preparation method and application thereof. The invention improves the theoretical capacity of the material by doping sulfur element, and simultaneously improves the content of nickel element to enlarge the potential window of the material, thereby improving the capacity and energy density of the battery.
A preparation method of a nanometer petal-shaped nickel-cobalt-molybdenum ternary metal sulfide comprises the following steps:
s1, dissolving ammonium molybdate tetrahydrate, nickel nitrate hexahydrate and cobalt nitrate hexahydrate in deionized water, and after completely and uniformly dissolving, adding sulfur powder and completely dispersing to form a uniform colloidal solution;
s2, adding hydrazine hydrate into the colloidal solution, fully stirring, and then transferring to an oven for solvothermal reaction;
and S3, washing the product of the solvothermal reaction with alcohol and water in sequence, alternately washing, drying, and transferring to a high-temperature tube furnace for high-temperature treatment to finally obtain the nano petal-shaped ternary metal sulfide material.
Further, after the sulfur powder is added in the step S1, the sulfur powder is completely dispersed in a continuous ultrasonic dispersion, stirring and heating mode, wherein the ultrasonic dispersion time is 0.5-1h, the stirring time is 0.5-3h, and the temperature is increased to 50-100 ℃.
Further, in the step S1, the mass ratio of ammonium molybdate tetrahydrate, nickel nitrate hexahydrate and cobalt nitrate hexahydrate is 1-3: 0.5-1.5: 0.2-1.1; the mass-to-volume ratio (g/ml) of ammonium molybdate tetrahydrate and deionized water is 1-3: 10-40 parts of; the mass ratio of ammonium molybdate tetrahydrate to sulfur powder is 1-3: 0.2-1.1.
Further, in the step S2, adding hydrazine hydrate into the colloidal solution and fully stirring until the color of the mixed solution is changed from light yellow to complete orange-red, and then transferring the mixed solution into an oven for solvothermal reaction; the volume ratio of the hydrazine hydrate to the deionized water is 5-20: 10-40.
Further, in the step S2, the temperature of the solvothermal reaction is 80-240 ℃, and the time is 10-40 h; the inner container of the oven is made of polytetrafluoroethylene.
Further, the high-temperature treatment in step S3 is performed in a reducing gas atmosphere; the high-temperature treatment comprises sintering and calcining, wherein the sintering temperature is 500-700 ℃, and the time is 2-6 h; the calcining temperature is 500-900 ℃, the time is 1-6h, and the heating rate is 1-10 ℃/min.
In a further scheme, the reducing gas is hydrogen or argon-hydrogen mixed gas, and the volume percentage of the hydrogen in the argon-hydrogen mixed gas is 2-10%.
Further, the yield of the ternary metal sulfide material in the step S3 is 60-90%.
The second invention aims to provide the nanometer petal-shaped nickel-cobalt-molybdenum ternary metal sulfide prepared by the preparation method.
The third purpose of the invention is to provide the application of the nano petal-shaped nickel-cobalt-molybdenum ternary metal sulfide, wherein the nano petal-shaped nickel-cobalt-molybdenum ternary metal sulfide is used as a positive electrode material of a lithium ion battery.
In the calcining process, the heating rate can influence the effect of reducing the precursor, if the heating rate is too high, the precursor mixture is heated unevenly, and meanwhile, the contact time of the precursor mixture and hydrogen is shortened, so that the internal reaction cannot be fully carried out, and the ideal effect cannot be achieved, therefore, the heating rate is controlled to be 1-10 ℃/min, and preferably 2 ℃/min.
Because the elemental sulfur has higher theoretical capacity (1675 mAh g-1), the invention aims to greatly improve the capacity of the anode material and improve the limitation of poor conductivity and stability of the single-sulfur electrode by preparing the nickel-cobalt-molybdenum ternary metal sulfide; meanwhile, the novel positive electrode material obtained by the invention has an obvious two-dimensional structure, and the migration rate of lithium ions is increased, so that the nano petal-shaped nickel-cobalt-molybdenum ternary metal sulfide used as the positive electrode material of the lithium-sulfur battery shows higher charge and discharge capacity, better cycle stability and energy density.
The preparation method is simple and easy to operate, has low cost, can be applied to various metal sulfide materials, has good adaptability, and is suitable for large-scale production.
The invention greatly improves the capacity of the metal material by regulating the shape of the material, the doping of sulfur element and other processes, and solves the problems of excessive side reaction, unstable structure, poor conductivity and the like of elemental sulfur as the lithium ion battery anode material, thereby being expected to greatly improve the energy density of the material and conforming to the energy development strategy of the new period of the country.
Drawings
Fig. 1 is an electron microscope image of a lithium-sulfur battery positive electrode material prepared from a nano petal-shaped nickel-cobalt-molybdenum ternary metal sulfide of example 2 of the present invention;
fig. 2 shows the charge-discharge performance and the cycle stability of the lithium-sulfur battery positive electrode material prepared from the nano petal-shaped nickel-cobalt-molybdenum ternary metal sulfide and the conventional nickel-cobalt-molybdenum ternary metal sulfide of example 3 of the present invention.
Detailed Description
The technical solution of the present invention will be described in detail below with reference to specific examples.
Example 1
S1, mixing ammonium molybdate tetrahydrate, nickel nitrate hexahydrate and cobalt nitrate hexahydrate in a mass ratio of 1: 1.5: 0.2 is dissolved in deionized water, after being completely and uniformly dissolved, sulfur powder is added, and the mixture is continuously ultrasonically dispersed for 1 hour and stirred for 3 hours, and then the temperature is raised to 100 ℃, so that the mixture is completely dispersed to form uniform colloidal solution; wherein the mass volume ratio (g/ml) of ammonium molybdate tetrahydrate, sulfur powder and deionized water is 1: 1.1: 10;
s2, adding hydrazine hydrate into the colloidal solution, fully stirring until the color of the mixed solution is changed from light yellow to complete orange red, then transferring the mixed solution into an oven with a liner made of polytetrafluoroethylene, and carrying out solvothermal reaction for 10 hours at the temperature of 240 ℃; the volume ratio of the hydrazine hydrate to the deionized water is 20: 40.
S3, sequentially washing the product of the solvothermal reaction with alcohol and water alternately, drying, transferring to a high-temperature tube furnace, and performing high-temperature treatment in a reducing gas atmosphere to finally obtain a nano petal-shaped ternary metal sulfide material; the high-temperature treatment comprises sintering and calcining, wherein the sintering temperature is 700 ℃, and the time is 2 hours; the calcining temperature is 500 ℃, the time is 6h, and the heating rate is 5 ℃/min.
In a further scheme, the reducing gas is hydrogen or argon-hydrogen mixed gas, and the volume percentage of the hydrogen in the argon-hydrogen mixed gas is 10%; the yield of the nickel-cobalt-molybdenum ternary metal sulfide material is 60-90%.
Example 2
S1, mixing ammonium molybdate tetrahydrate, nickel nitrate hexahydrate and cobalt nitrate hexahydrate in a mass ratio of 2: 1.5: 1.1 dissolving in deionized water, adding sulfur powder after completely dissolving uniformly, dispersing for 1h through continuous ultrasonic, stirring for 3h, and then heating to 100 ℃ to ensure that the sulfur powder is completely dispersed to form uniform colloidal solution; wherein the mass volume ratio (g/ml) of ammonium molybdate tetrahydrate, sulfur powder and deionized water is 2: 0.8: 3;
s2, adding hydrazine hydrate into the colloidal solution, fully stirring until the color of the mixed solution is changed from light yellow to complete orange red, then transferring the mixed solution into an oven with a liner made of polytetrafluoroethylene, and carrying out solvothermal reaction for 10-40h at the temperature of 240 ℃; the volume ratio of the hydrazine hydrate to the deionized water is 15: 36.
S3, sequentially washing the product of the solvothermal reaction with alcohol and water alternately, drying, transferring to a high-temperature tube furnace, and performing high-temperature treatment in a reducing gas atmosphere to finally obtain a nano petal-shaped ternary metal sulfide material; the high-temperature treatment comprises sintering and calcining, wherein the sintering temperature is 700 ℃, and the time is 6 hours; the calcining temperature is 900 ℃, the time is 1h, and the heating rate is 10 ℃/min.
In a further scheme, the reducing gas is hydrogen or argon-hydrogen mixed gas, and the volume percentage of the hydrogen in the argon-hydrogen mixed gas is 10%; the yield of the nickel-cobalt-molybdenum ternary metal sulfide material is 60-90%.
The morphology characteristics of the lithium-sulfur battery positive electrode material prepared from the nano-petal nickel-cobalt-molybdenum ternary metal sulfide prepared in example 2 were examined, and the structure thereof is shown in fig. 1 below. As shown in fig. 1, the nano petal-shaped nickel-cobalt-molybdenum ternary metal sulfide as the positive electrode material of the lithium-sulfur battery has a porous structure and a large specific surface area.
Example 3
S1, mixing ammonium molybdate tetrahydrate, nickel nitrate hexahydrate and cobalt nitrate hexahydrate in a mass ratio of 1.7: 0.9: 0.8 is dissolved in deionized water, after the solution is completely and uniformly dissolved, the sulfur powder is added, and the solution is dispersed for 0.8 hour and stirred for 2.4 hours by continuous ultrasonic, and then the temperature is raised to 80 ℃ to ensure that the solution is completely dispersed to form uniform colloidal solution; wherein the mass-volume ratio (g/ml) of ammonium molybdate tetrahydrate, sulfur powder and deionized water is 1.7: 0.7: 24;
s2, adding hydrazine hydrate into the colloidal solution, fully stirring until the color of the mixed solution is changed from light yellow to complete orange red, then transferring the mixed solution into an oven with a liner made of polytetrafluoroethylene, and carrying out solvothermal reaction for 10-40h at the temperature of 80-240 ℃; the volume ratio of the hydrazine hydrate to the deionized water is 14: 27.
S3, sequentially washing the product of the solvothermal reaction with alcohol and water alternately, drying, transferring to a high-temperature tube furnace, and performing high-temperature treatment in a reducing gas atmosphere to finally obtain a nano petal-shaped ternary metal sulfide material; the high-temperature treatment comprises sintering and calcining, wherein the sintering temperature is 600 ℃, and the time is 4 hours; the calcining temperature is 800 ℃, the time is 3h, and the heating rate is 5 ℃/min.
In a further scheme, the reducing gas is hydrogen or argon-hydrogen mixed gas, and the volume percentage of the hydrogen in the argon-hydrogen mixed gas is 7%; the yield of the nickel-cobalt-molybdenum ternary metal sulfide material is 60-90%.
Under the condition that the current is 0.2A g-1, the charge and discharge performance and the cycle stability of the lithium-sulfur battery cathode material respectively prepared from the nano petal-shaped nickel-cobalt-molybdenum ternary metal sulfide obtained in example 3 and the existing nickel-cobalt-molybdenum ternary metal sulfide are detected, and the results are shown in the following fig. 2. As can be seen from fig. 2, the charge and discharge performance and the cycle stability of the nano petal-shaped nickel-cobalt-molybdenum ternary metal sulfide as the lithium ion battery anode material are shown in the left diagram in fig. 2, and the nano petal-shaped nickel-cobalt-molybdenum ternary metal sulfide has higher charge and discharge capacity and cycle stability. And has much better charge-discharge capacity and cycle stability than the existing nickel-cobalt-molybdenum ternary metal sulfide used as the anode material (right figure) of the lithium ion battery.
Example 4
S1, mixing ammonium molybdate tetrahydrate, nickel nitrate hexahydrate and cobalt nitrate hexahydrate in a mass ratio of 1.1: 0.8: 0.9 is dissolved in deionized water, after the solution is completely and uniformly dissolved, the sulfur powder is added, and the solution is dispersed for 0.5h and stirred for 0.5h through continuous ultrasonic, and then the temperature is raised to 50 ℃ to ensure that the solution is completely dispersed to form uniform colloidal solution; wherein the mass-volume ratio (g/ml) of ammonium molybdate tetrahydrate, sulfur powder and deionized water is 1.1: 0.5: 10;
s2, adding hydrazine hydrate into the colloidal solution, fully stirring until the color of the mixed solution is changed from light yellow to complete orange red, then transferring the mixed solution into an oven with a liner made of polytetrafluoroethylene, and carrying out solvothermal reaction for 10-40h at the temperature of 80-240 ℃; the volume ratio of the hydrazine hydrate to the deionized water is 6: 13.
S3, sequentially washing the product of the solvothermal reaction with alcohol and water alternately, drying, transferring to a high-temperature tube furnace, and performing high-temperature treatment in a reducing gas atmosphere to finally obtain a nano petal-shaped ternary metal sulfide material; the high-temperature treatment comprises sintering and calcining, wherein the sintering temperature is 500 ℃, and the time is 2 hours; the calcining temperature is 500 ℃, the time is 6h, and the heating rate is 1 ℃/min.
In a further scheme, the reducing gas is hydrogen or argon-hydrogen mixed gas, and the volume percentage of the hydrogen in the argon-hydrogen mixed gas is 2%; the yield of the nickel-cobalt-molybdenum ternary metal sulfide material is 60-90%.
Example 5
S1, mixing ammonium molybdate tetrahydrate, nickel nitrate hexahydrate and cobalt nitrate hexahydrate in a mass ratio of 1.7: 0.8: 0.9 is dissolved in deionized water, after the solution is completely and uniformly dissolved, the sulfur powder is added, and the solution is dispersed for 0.8 hour and stirred for 2.4 hours by continuous ultrasonic, and then the temperature is raised to 80 ℃ to ensure that the solution is completely dispersed to form uniform colloidal solution; wherein the mass-volume ratio (g/ml) of ammonium molybdate tetrahydrate, sulfur powder and deionized water is 1.7: 0.8: 10;
s2, adding hydrazine hydrate into the colloidal solution, fully stirring until the color of the mixed solution is changed from light yellow to complete orange red, then transferring the mixed solution into an oven with a liner made of polytetrafluoroethylene, and carrying out solvothermal reaction for 10-40h at the temperature of 80-240 ℃; the volume ratio of the hydrazine hydrate to the deionized water is 14: 27.
S3, sequentially washing the product of the solvothermal reaction with alcohol and water alternately, drying, transferring to a high-temperature tube furnace, and performing high-temperature treatment in a reducing gas atmosphere to finally obtain a nano petal-shaped ternary metal sulfide material; the high-temperature treatment comprises sintering and calcining, wherein the sintering temperature is 600 ℃, and the time is 4 hours; the calcining temperature is 800 ℃, the time is 4h, and the heating rate is 3 ℃/min.
In a further scheme, the reducing gas is hydrogen or argon-hydrogen mixed gas, and the volume percentage of the hydrogen in the argon-hydrogen mixed gas is 7%; the yield of the nickel-cobalt-molybdenum ternary metal sulfide material is 60-90%.
The above description is only for the preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art should be considered to be within the technical scope of the present invention, and the technical solutions and the inventive concepts thereof according to the present invention should be equivalent or changed within the scope of the present invention.
Claims (9)
1. A preparation method of nanometer petal-shaped nickel-cobalt-molybdenum ternary metal sulfide is characterized by comprising the following steps: the method comprises the following steps:
s1, dissolving ammonium molybdate tetrahydrate, nickel nitrate hexahydrate and cobalt nitrate hexahydrate in deionized water, and after completely and uniformly dissolving, adding sulfur powder and completely dispersing to form a uniform colloidal solution;
s2, adding hydrazine hydrate into the colloidal solution, fully stirring until the color of the mixed solution is changed from light yellow to complete orange red, and then transferring the mixed solution into an oven for solvothermal reaction;
s3, washing the product of the solvothermal reaction with alcohol and water in sequence, alternately washing, drying, transferring to a high-temperature tube furnace, and performing high-temperature treatment in a reducing gas atmosphere to finally obtain a nano petal-shaped ternary metal sulfide material; the high-temperature treatment comprises sintering and calcining, wherein the sintering temperature is 500-700 ℃, and the time is 2-6 h; the calcining temperature is 500-900 ℃, the time is 1-6h, and the heating rate is 1-10 ℃/min.
2. The method of claim 1, wherein: and S1, completely dispersing the sulfur powder by continuous ultrasonic dispersion, stirring and heating, wherein the ultrasonic dispersion time is 0.5-1h, the stirring time is 0.5-3h, and the temperature is increased to 50-100 ℃.
3. The method of claim 1, wherein: in the step S1, the mass ratio of ammonium molybdate tetrahydrate, nickel nitrate hexahydrate and cobalt nitrate hexahydrate is 1-3: 0.5-1.5: 0.2-1.1; the mass volume ratio g of the ammonium molybdate tetrahydrate to the deionized water is as follows: mL is 1-3: 10-40 parts of; the mass ratio of ammonium molybdate tetrahydrate to sulfur powder is 1-3: 0.2-1.1.
4. The method of claim 1, wherein: in the step S2, the volume ratio of the hydrazine hydrate to the deionized water is 5-20: 10-40.
5. The method of claim 1, wherein: in the step S2, the temperature of the solvothermal reaction is 80-240 ℃, and the time is 10-40 h; the inner container of the oven is made of polytetrafluoroethylene.
6. The method of claim 1, wherein: the reducing gas is hydrogen or argon-hydrogen mixed gas, and the volume percentage of the hydrogen in the argon-hydrogen mixed gas is 2-10%.
7. The method of claim 1, wherein: the yield of the ternary metal sulfide material in step S3 is 60-90%.
8. The nickel-cobalt-molybdenum ternary metal sulfide in a nanometer petal shape prepared by the preparation method of claim 1.
9. The use of nano-petal nickel cobalt molybdenum ternary metal sulfide as claimed in claim 8, wherein: the nanometer petal-shaped nickel-cobalt-molybdenum ternary metal sulfide is used as a positive electrode material of a lithium ion battery.
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| "A NiMoS flower-like structure with self-assembled nanosheets as high-performance hydrodesulfurization catalysts";Weikun Lai，et al.;《Nanoscale》;20160112;第8卷;第3823-3833页 * |
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