CN114420916A - Lithium-sulfur battery positive electrode material and preparation method and application thereof - Google Patents

Lithium-sulfur battery positive electrode material and preparation method and application thereof Download PDF

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CN114420916A
CN114420916A CN202210078802.9A CN202210078802A CN114420916A CN 114420916 A CN114420916 A CN 114420916A CN 202210078802 A CN202210078802 A CN 202210078802A CN 114420916 A CN114420916 A CN 114420916A
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lithium
sulfur battery
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CN114420916B (en
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蔡道平
王亚光
廖茹忻
傅俊杰
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Fuzhou University
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    • H01—ELECTRIC ELEMENTS
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    • H01M4/38—Selection of substances as active materials, active masses, active liquids of elements or alloys
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M10/00—Secondary cells; Manufacture thereof
    • H01M10/05—Accumulators with non-aqueous electrolyte
    • H01M10/052—Li-accumulators
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00—Electrodes
    • H01M4/02—Electrodes composed of, or comprising, active material
    • H01M4/36—Selection of substances as active materials, active masses, active liquids
    • H01M4/38—Selection of substances as active materials, active masses, active liquids of elements or alloys
    • H01M4/381—Alkaline or alkaline earth metals elements
    • H01M4/382—Lithium
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
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    • H01M4/02—Electrodes composed of, or comprising, active material
    • H01M4/36—Selection of substances as active materials, active masses, active liquids
    • H01M4/58—Selection of substances as active materials, active masses, active liquids of inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy; of polyanionic structures, e.g. phosphates, silicates or borates
    • H01M4/581—Chalcogenides or intercalation compounds thereof
    • H01M4/5815—Sulfides
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Abstract

The invention discloses a lithium-sulfur battery positive electrode material and a preparation method and application thereof, belonging to the field of preparation of lithium-sulfur battery electrode materials; wherein the positive electrode material of the lithium-sulfur battery comprises VN @ Co3ZnC @ NCNTs composite material and sulfur, VN @ Co3The ZnC @ NCNTs composite material comprises VN and Co3ZnC and nitrogen-doped carbon nanotubes; the lithium-sulfur battery prepared by the lithium-sulfur battery cathode material has obviously improved electrochemical performance, and the lithium-sulfur battery cathode material is simple to prepare, simple and convenient in battery assembly process and capable of reducing cost.

Description

Lithium-sulfur battery positive electrode material and preparation method and application thereof
Technical Field
The invention belongs to the field of preparation of electrode materials for lithium-sulfur batteries, and particularly relates to a positive electrode material VN @ Co for a lithium-sulfur battery3ZnC @ NCNTs @ S and a preparation method and application thereof.
Background
In the 21 st century, high performance electrochemical energy storage devices are continuously sought after. In addition to commercial lithium ion batteries, lithium sulfur batteries have become one of the most promising batteries for next generation energy storage systems by virtue of their high theoretical specific capacity (1675 mAh/g) and overwhelming energy density (2600 Wh/kg). The electrochemical reaction of lithium-sulfur batteries is based on sulfur (S)8) Lithium polysulfide (Li)2SxX = 4-8) and lithium sulfide (Li)2S2And Li2S) can be reversed. However, the commercialization of lithium sulfur batteries is also facing many obstacles: (1) the electric conductivity of sulfur and lithium sulfide is low, and the redox reaction kinetics is slow; (2) shuttling effects resulting from dissolution and diffusion of soluble lithium polysulphides (LiPSs); (3) upon lithiation, sulfur undergoes a significant volume expansion (up to 80%). Therefore, the lithium-sulfur battery has the problems of low utilization rate of sulfur, poor cycle stability, low rate performance and the like.
The positive electrode material with reasonable design and high quality can effectively solve the defects of the lithium-sulfur battery. Polar materials include metals, metal oxides, sulfides, nitrides, phosphides, carbides, etc., as compared to non-polar materials, and have received attention for their strong chemisorption of lithium polysulfides. Among them, transition metal nitrides have attracted attention because of their unique electronic structure, high electrical conductivity, superior catalytic activity and good chemical stability. To date, there are a number of transition metal nitrides (e.g., Co)4N、Fe2N, MoN, VN, TiN, etc.) have proven to be sulfur host materials. However, due to their low specific surface area, they interact weakly with lithium polysulfides and are not ideal host materials for sulfur. To further improve the performance of transition metal nitrides, transition metal nitrides have been combined with strong LiPSs adsorption materials.
Furthermore, the host material of sulfur is a powder material which is easy to prepare in large scale, and an insulating polymer binder and a conductive additive are required in the preparation process of the electrode.
Disclosure of Invention
In view of the above-mentioned proposalThe invention aims to provide a positive electrode material VN @ Co of a lithium-sulfur battery3The positive electrode material of the lithium-sulfur battery comprises VN @ Co3ZnC @ NCNTs composite material and sulfur, VN @ Co3ZnC @ NCNTs comprises VN and Co3ZnC and nitrogen-doped carbon nano-tubes, wherein VN is a nano-sheet with the width of 50 nm and the length of 1-2 mu m, and the diameter of the nitrogen-doped carbon nano-tube is 20 nm. By applying the cathode material to the lithium-sulfur battery, the electrode of the lithium-sulfur battery is simple in preparation process and has excellent rate performance and cycling stability.
In order to achieve the purpose, the invention adopts the following technical scheme:
positive electrode material VN @ Co of lithium-sulfur battery3The preparation method of ZnC @ NCNTs/S comprises the following steps:
(1) adding ammonium metavanadate into deionized water, stirring and dissolving, then adding cobalt dichloride into the solution, stirring and dissolving at room temperature, then adding hexamethylenetetramine, placing the solution on a water bath kettle for water bath reaction, centrifuging the reacted solution, washing with absolute ethyl alcohol and deionized water for multiple times, and then placing the solution in an oven for drying to obtain Co2V2O7；
(2) Adding PVP (polyvinylpyrrolidone) and zinc nitrate hexahydrate into methanol, and uniformly stirring to obtain a solution A; adding 1, 2-dimethyl imidazole into methanol, uniformly stirring to obtain a solution B, and drying the Co obtained in the step (1)2V2O7Placing the solution A into the solution A, slowly stirring by magnetic force, simultaneously dripping the solution B into the solution A for reaction, centrifuging the solution after the reaction is finished, cleaning the solution with absolute ethyl alcohol, and finally drying the washed product to obtain Co2V2O7@ZIF-8；
(3) Putting the dried product obtained in the step (2) into a porcelain boat, flatly laying melamine in another porcelain boat, and then placing the two porcelain boats into argon-hydrogen (Ar +5% H)2) Nitriding in a protected tube furnace, and naturally cooling to obtain VN @ Co3ZnC@NCNTs；
(4) Nitriding step (3)Uniformly mixing the product and sulfur powder, then putting the mixture into a small bottle, sealing the bottle, carrying out a melting reaction in an oven, and naturally cooling the bottle to obtain the positive electrode material VN @ Co of the lithium-sulfur battery3ZnC@NCNTs@S。
Further, the preparation method specifically comprises the following steps:
(1) adding 0.1-1.0 g of ammonium metavanadate into 20-200 mL of deionized water, stirring for dissolving, then adding cobalt dichloride into the solution, stirring for dissolving at room temperature, then adding 0.6-6 g of hexamethylenetetramine, placing the solution on a water bath kettle for water bath reaction at the reaction temperature of 40-100 ℃ for 2-20 hours, centrifuging the reacted solution, washing with absolute ethyl alcohol and deionized water for multiple times, and then placing the solution in an oven for drying to obtain Co2V2O7；
(2) Adding 0.5-5 g of PVP and 0.36-3.6 g of zinc nitrate hexahydrate into 10-100 mL of methanol, and uniformly stirring to obtain a solution A; adding 0.4-3.2 g of 1, 2-dimethyl imidazole into 10-100 mL of methanol, uniformly stirring to obtain a solution B, and drying the Co obtained in the step (1)2V2O7Putting the solution A into the solution A, slowly stirring the solution A by magnetic force, dripping the solution B into the solution A, reacting for 5 to 50 minutes, centrifuging the reacted solution, cleaning the solution by absolute ethyl alcohol, and finally drying the washed product to obtain Co2V2O7@ZIF-8；
(3) 50-500 mg of Co2V2O7@ ZIF-8 is placed in one porcelain boat, 1-10 g of melamine is flatly laid in the other porcelain boat, and then the two porcelain boats are placed in argon (Ar +5% H)2) And nitriding in a protected tube furnace, wherein the reaction temperature is 300-1000 ℃, the heat preservation time is 1-10 hours, and the heating rate is 2-25 ℃/min. After the mixture is naturally cooled, obtaining VN @ Co3ZnC@NCNTs；
(4) And (3) uniformly mixing 5-50 mg of the product nitrided in the step (3) with 90-900 mg of sulfur powder, then putting the mixture into a small bottle, sealing the bottle, and carrying out a melting reaction in an oven, wherein the reaction temperature is 75-300 ℃ and the reaction time is 6-60 hours. Naturally cooling to obtain the positive electrode material VN @ Co of the lithium-sulfur battery3ZnC@NCNTs@S。
The application comprises the following steps: positive electrode material VN @ Co of lithium-sulfur battery3Application of ZnC @ NCNTs @ S in assembling a lithium-sulfur battery.
The invention has the following remarkable advantages:
the invention provides a positive electrode material VN @ Co of a lithium-sulfur battery3A preparation method of ZnC @ NCNTs @ S. High-conductivity VN and NCNTs can accelerate electron transmission; polarity VN and Co3The ZnC material has strong physical/chemical adsorption on LiPSs so as to prevent a shuttle effect; VN and Co3ZnC can be used as a good electrocatalyst to accelerate the conversion of LiPSs, and the reaction kinetics and the efficient utilization of sulfur are improved. Therefore, the rate performance and the cycle performance of the lithium-sulfur battery assembled by the cathode material are obviously improved.
Drawings
Fig. 1 is an XRD diffraction pattern of the positive electrode material for lithium sulfur battery prepared in example 1;
FIG. 2 is a scanning electron micrograph of a positive electrode material for a lithium sulfur battery prepared according to example 1;
FIG. 3 is a cyclic voltammogram of the positive electrode material of the lithium sulfur battery prepared in example 1;
FIG. 4 is a graph showing the charge and discharge curves of the positive electrode material for a lithium sulfur battery prepared in example 1;
FIG. 5 is a scanning electron microscope image of the positive electrode material of the lithium sulfur battery prepared in comparative example 1;
fig. 6 is a graph comparing electrochemical properties of the cathode material of the lithium sulfur battery manufactured in example 1 and the cathode material of the lithium sulfur battery manufactured in comparative example 1.
Detailed Description
In order to make the aforementioned and other features and advantages of the invention more comprehensible, embodiments accompanied with figures are described in detail below. The method of the present invention is a method which is conventional in the art unless otherwise specified.
Example 1
Positive electrode material VN @ Co of lithium-sulfur battery3The preparation method of ZnC @ NCNTs @ S comprises the following specific steps:
(1) 0.25 g of ammonium metavanadate was added to 30 mL of deionized water, dissolved with stirring, and then 0.2 g of cobalt dichloride was added to the above solution, dissolved with stirring at room temperature, followed by addition ofAdding 2.4 g of hexamethylenetetramine, placing the solution on a water bath kettle for water bath reaction at the reaction temperature of 80 ℃ for 6 hours, centrifuging the reacted solution, washing the solution with absolute ethyl alcohol and deionized water for three times, and placing the washed solution in an oven for drying to obtain Co2V2O7；
(2) Adding 1g of PVP and 0.72 g of zinc nitrate hexahydrate into 20 mL of methanol, and uniformly stirring to obtain a solution A; adding 0.8 g of 1, 2-dimethylimidazole into 20 mL of methanol, uniformly stirring to obtain a solution B, and drying the Co obtained in the step (1)2V2O7Adding the solution B into the solution A, slowly stirring by magnetic force, dripping the solution B into the solution A, reacting at room temperature for 30 minutes, centrifuging the reacted solution, washing with absolute ethyl alcohol, and finally drying the washed product to obtain Co2V2O7@ZIF-8；
(3) Mixing 100 mg of Co2V2O7@ ZIF-8 was placed in one porcelain boat, 2 g melamine was spread in another porcelain boat, and then the two porcelain boats were placed in argon (Ar +5% H)2) Nitriding in a protected tube furnace at the reaction temperature of 600 ℃, keeping the temperature for 4 hours and raising the temperature at the rate of 10 ℃/min. After the mixture is naturally cooled, obtaining VN @ Co3ZnC@NCNTs。
(4) And (3) uniformly mixing 50 mg of the product nitrided in the step (3) and 180 mg of sulfur powder, then putting the mixture into a small bottle, sealing the bottle, and carrying out a melt reaction in an oven at the reaction temperature of 150 ℃ for 12 hours. Naturally cooling to obtain the positive electrode material VN @ Co of the lithium-sulfur battery3ZnC@NCNTs@S。
FIG. 2 is a scanning electron micrograph of a positive electrode material for a lithium sulfur battery prepared according to example 1; the graph shows that the carbon nano tubes are almost uniformly paved, the tubes are uniform in thickness, the size diameter is about 20 nm, the growth is controllable, the appearance of the exposed internal hexagon can be obviously seen, and the appearance of the vanadium nitride on the surface can be maintained; FIG. 3 is a cyclic voltammogram of the positive electrode material of the lithium sulfur battery prepared in example 1; the curve exhibits a larger integrated area; FIG. 4 is a graph showing the charge and discharge curves of the positive electrode material for a lithium sulfur battery prepared in example 1; it can be seen from the figure that the charging and discharging platforms have a small vertical distance.
Example 2
Positive electrode material VN @ Co of lithium-sulfur battery3The preparation method of ZnC @ NCNTs @ S comprises the following specific steps:
(1) adding 0.5 g of ammonium metavanadate into 40 mL of deionized water, stirring and dissolving, then adding 0.2 g of cobalt dichloride into the solution, stirring and dissolving at room temperature, then adding 1.2 g of hexamethylenetetramine, placing the solution on a water bath kettle to perform water bath reaction at the reaction temperature of 80 ℃ for 4 hours, centrifuging the reacted solution, washing the solution with absolute ethyl alcohol and deionized water for multiple times, and then placing the solution in an oven for drying to obtain Co2V2O7；
(2) Adding 1g of PVP and 0.73 g of zinc nitrate hexahydrate into 20 mL of methanol, and uniformly stirring to obtain a solution A; adding 1.6 g of 1, 2-dimethylimidazole into 20 mL of methanol, uniformly stirring to obtain a solution B, and drying the Co obtained in the step (1)2V2O7Adding the solution B into the solution A, slowly stirring by magnetic force, dripping the solution B into the solution A, reacting at room temperature for 10 minutes, centrifuging the reacted solution, washing with absolute ethyl alcohol, and finally drying the washed product to obtain Co2V2O7@ZIF-8；
(3) Mixing 200 mg of Co2V2O7@ ZIF-8 was placed in one porcelain boat, 3 g melamine was spread in another porcelain boat, and then the two porcelain boats were placed in argon (Ar +5% H)2) Nitriding in a protected tube furnace at the reaction temperature of 600 ℃, keeping the temperature for 2 hours and raising the temperature at the rate of 5 ℃/min. After the mixture is naturally cooled, obtaining VN @ Co3ZnC@NCNTs。
(4) And (3) uniformly mixing 30 mg of the product nitrided in the step (3) with 108 mg of sulfur powder, then putting the mixture into a small bottle, sealing the bottle, and carrying out a melt reaction in an oven at the reaction temperature of 150 ℃ for 8 hours. Naturally cooling to obtain the positive electrode material VN @ Co of the lithium-sulfur battery3ZnC@NCNTs@S。
Electrochemical performance test
VN @ Co prepared by the method3ZnC@NCNTs @ S as the positive electrode, lithium sheet as the negative electrode, commercial separator Celgard 2400 as the separator, and the cell was assembled in a glove box using a CR2032 cell casing. The lithium sulfur battery shows that the capacity of the electrode material prepared in example 1 is 1300 mAh/g under the current density of 0.1C, and the electrode material has higher specific capacity.
Comparative example 1
The method for preparing the lithium-sulfur battery positive electrode material comprises the following steps:
(1) adding 0.25 g of ammonium metavanadate into 30 mL of deionized water, stirring and dissolving, then adding 0.2 g of cobalt dichloride into the solution, stirring and dissolving at room temperature, then adding 2.4 g of hexamethylenetetramine, placing the solution on a water bath kettle to perform water bath reaction at the reaction temperature of 80 ℃ for 6 hours, centrifuging the reacted solution, washing the solution with absolute ethyl alcohol and deionized water for multiple times, and then placing the solution in an oven for drying to obtain Co2V2O7；
(2) Mixing 100 mg of Co2V2O7Placing into a porcelain boat, spreading 1g melamine in another porcelain boat, and placing into argon (Ar +5% H)2) Nitriding in a protected tube furnace at the reaction temperature of 600 ℃, keeping the temperature for 4 hours and raising the temperature at the rate of 10 ℃/min. After the VN @ NCNTs/Co is naturally cooled, VN @ NCNTs/Co is obtained, which means that carbon tubes are generated on the VN substrate, and Co particles are arranged in the carbon tubes.
(3) And (3) uniformly mixing 50 mg of the product nitrided in the step (2) and 180 mg of sulfur powder, then putting the mixture into a small bottle, sealing the bottle, and carrying out a melt reaction in an oven at the reaction temperature of 150 ℃ for 12 hours. And naturally cooling to obtain the positive electrode material VN @ NCNTs/Co @ S of the lithium-sulfur battery.
Fig. 5 is a scanning electron microscope image of the positive electrode material of the lithium sulfur battery prepared in comparative example 1. As can be seen from the figure, the overall morphology of the nitrided material without MOF growth is disordered, the carbon nanotubes are thick and overlong, the size diameter is about 100 nm, the surface of the material is tightly covered, and the internal vanadium nitride can not maintain the original hexagonal morphology.
The electrochemical performance test of the positive electrode material of the lithium-sulfur battery prepared by the method is carried out according to the same method, and the capacity of the electrode material prepared by the comparative example 1 is 1180 mAh/g under the current density of 0.1C, while the capacity of the electrode material prepared by the comparative example 1 is 1300 mAh/g and has larger Cyclic Voltammetry (CV) area under the same condition. The comparison shows that the specific capacity of the electrode material is effectively improved by the material obtained by growing and nitriding the MOF.
The above description is only a preferred embodiment of the present invention, and all equivalent changes and modifications made in accordance with the claims of the present invention should be covered by the present invention.

Claims (10)

1. A preparation method of a lithium-sulfur battery positive electrode material is characterized by comprising the following steps: the method comprises the following steps:
(1) adding ammonium metavanadate into deionized water, stirring and dissolving, then adding cobalt dichloride into the solution, stirring and dissolving at room temperature, then adding hexamethylenetetramine, placing the solution on a water bath kettle for water bath reaction, centrifuging the reacted solution, washing with absolute ethyl alcohol and deionized water for multiple times, and then placing the solution in an oven for drying to obtain Co2V2O7；
(2) Adding PVP and zinc nitrate hexahydrate into a methanol solvent, and uniformly stirring to obtain a solution A; adding 1, 2-dimethyl imidazole into a methanol solvent, uniformly stirring to obtain a solution B, and drying the Co obtained in the step (1)2V2O7Placing the solution A into the solution A, slowly stirring by magnetic force, simultaneously dripping the solution B into the solution A for reaction, centrifuging the solution after the reaction is finished, cleaning the solution with absolute ethyl alcohol, and finally drying the washed product to obtain Co2V2O7@ZIF-8；
(3) Putting the dried product in the step (2) into a porcelain boat, flatly spreading melamine in another porcelain boat, then putting the two porcelain boats into a tube furnace protected by argon and hydrogen for nitriding, and naturally cooling;
(4) and (3) uniformly mixing the nitriding product obtained in the step (3) with sulfur powder, then placing the mixture into a small bottle, sealing the bottle, carrying out a melting reaction in an oven, and naturally cooling the bottle to obtain the lithium-sulfur battery positive electrode material.
2. The method of claim 1, wherein: in the step (1), the mass of the ammonium metavanadate is 0.1-1.0 g, the mass of the cobalt dichloride is 0.05-0.5 g, and the mass of the hexamethylenetetramine is 0.6-6 g.
3. The method of claim 1, wherein: in the step (1), the water bath reaction temperature is 40-100 ℃, and the reaction time is 2-20 hours.
4. The method of claim 1, wherein: in the step (2), the mass of PVP is 0.5-5 g, the mass of zinc nitrate hexahydrate is 0.36-3.6 g, and Co is2V2O7The mass is 5-50 g, the mass of 1, 2-dimethyl imidazole is 0.4-3.2 g, and the reaction time is 5-50 minutes.
5. The method of claim 1, wherein: in the step (3), the mass of the melamine is 1-10 g, and Co is2V2O7The mass of @ ZIF-8 is 50-500 mg.
6. The method of claim 1, wherein: in the step (3), the nitriding temperature is 300-1000 ℃, the heating rate is 2-25 ℃/min, and the heat is preserved for 1-10 h.
7. The method of claim 1, wherein: in the step (4), the mass of the sulfur powder is 90-900 mg, and the mass of the nitriding product is 5-50 g.
8. The method of claim 1, wherein: in the step (4), the melting reaction temperature is 75-300 ℃, and the reaction time is 6-60 hours.
9. A positive electrode material for a lithium-sulfur battery produced by the production method according to any one of claims 1 to 8.
10. Use of the lithium sulfur battery positive electrode material of claim 9 in assembling a lithium sulfur battery.
CN202210078802.9A 2022-01-24 2022-01-24 Positive electrode material of lithium-sulfur battery, and preparation method and application thereof Active CN114420916B (en)

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CN109713282A (en) * 2018-12-29 2019-05-03 珠海光宇电池有限公司 A kind of lithium sulfur battery anode material and preparation method thereof and lithium-sulfur cell
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