CN114824204A - Preparation method of carbon-coated cobalt-nickel binary transition metal sulfide negative electrode material - Google Patents
Preparation method of carbon-coated cobalt-nickel binary transition metal sulfide negative electrode material Download PDFInfo
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- CN114824204A CN114824204A CN202210393561.7A CN202210393561A CN114824204A CN 114824204 A CN114824204 A CN 114824204A CN 202210393561 A CN202210393561 A CN 202210393561A CN 114824204 A CN114824204 A CN 114824204A
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- 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
- H01M4/362—Composites
- H01M4/366—Composites as layered products
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- 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
- H01M4/58—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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- 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
- H01M4/58—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
- H01M4/583—Carbonaceous material, e.g. graphite-intercalation compounds or CFx
- H01M4/587—Carbonaceous material, e.g. graphite-intercalation compounds or CFx for inserting or intercalating light metals
Abstract
The invention relates to a preparation method of a carbon-coated bimetallic sulfide lithium ion battery cathode material. The bimetallic sulfide Co9S8@ Ni3S2 is directly prepared by a solvothermal method, and then coated by polydopamine, and then calcined to obtain the NixCoyS @ C (x: y is 1: 1-2) material. The prepared carbon-coated bimetallic sulfide NixCoyS @ C material is used as a lithium ion battery cathode material, and the volume expansion of the transition metal sulfide used as the lithium ion battery cathode material is improved by the synergistic effect of bimetallic sulfide heterostructures and the carbon-coated structure, so that the cycle performance of the battery is improved.
Description
Technical Field
The invention belongs to the technical field of preparation of lithium ion battery electrode materials, and particularly relates to a preparation method of a carbon-coated cobalt-nickel binary transition metal sulfide negative electrode material.
Background
With the increasing global energy crisis and environmental problems, people are beginning to find new environmentally friendly energy sources to solve these problems. The development of new energy technology cannot leave safe and environment-friendly energy storage equipment. Because of the advantages of small volume, large capacity, environmental friendliness, portability and the like, the lithium ion battery has been widely used in social life as a new energy storage device. The lithium ion battery is composed of a positive electrode material, a negative electrode material, a diaphragm, an electrolyte and other accessories. The cathode material is a key material of the lithium ion battery. Graphite materials are currently the most widely used commercial anode materials. However, the use of graphite negative electrode materials has reached its theoretical capacity (372mAh g) -1 ) The limit of (c). With the demand of people for high energy density lithium ion batteries, the development of a new generation of lithium ion battery cathode material is imminent.
Compared with carbon materials such as graphite, the transition metal sulfide provides more active sites for Li + insertion and extraction, and has excellent energy storage performance. Among transition metal sulfides, CoS is a typical representative thereof. The theoretical specific capacity of the material reaches up to 590mAh/g, and the material is a new generation of lithium ion battery cathode material with huge potential. However, CoS as a lithium ion battery cathode material has large volume change, sharply attenuated specific capacity and poor cycle performance in the charging and discharging processes; in addition, CoS has poor conductivity compared to carbon materials.
In order to solve the above problems, measures often taken by researchers include: firstly, other metals are introduced, the problem of volume expansion in the charging and discharging process is relieved by utilizing the synergistic effect of the two metals, and the electrochemical performance of the battery is improved; the other method is to coat the metal sulfide with a carbon-based material, so that the conductivity of the sulfide is enhanced, and the volume expansion problem of the sulfide can be relieved.
Disclosure of Invention
The invention provides a lithium ion battery cathode material with a carbon-coated bimetallic sulfide heterostructure and a preparation method thereof. On one hand, nickel is introduced to improve the electrochemical performance by utilizing the synergistic effect of two metals, and on the other hand, the coating of the carbon-based material enhances the conductivity of the material on the basis of further relieving the volume expansion.
In order to achieve the expected effect, the invention adopts the following technical scheme:
a preparation method of a carbon-coated cobalt-nickel binary transition metal sulfide negative electrode material comprises the following steps:
(1) preparation of NixCoyS:
mixing nickel nitrate hexahydrate, cobalt nitrate hexahydrate, urea and thiourea according to a molar ratio of 1:2: 2-8: 4-10, adding 60mL of deionized water, ultrasonically stirring until the solution is uniform, placing the solution in an oven for heating reaction to obtain a black precipitate, performing suction filtration to collect a product, repeatedly washing the product with deionized water, and placing the product in the oven for drying to obtain a NixCoyS material;
(2) synthesis of NixCoyS @ PDA:
dispersing the NixCoyS material obtained in the step (1) in 100mL of Tris-HCl buffer aqueous solution, adding dopamine hydrochloride after stirring and mixing uniformly, then washing and collecting a precipitate product, repeatedly washing the product with deionized water, and then placing the product in an oven for drying to obtain a NixCoyS @ PDA product;
(3) synthesis of NixCoyS @ C:
and (3) placing the NixCoyS @ PDA precursor obtained in the step (2) into a tubular furnace for calcining, and cooling to room temperature to obtain the NixCoyS @ C negative electrode material.
Further, the reaction temperature in the step (1) is 180-200 ℃, and the reaction time is 12-24 hours.
Further, the pH of the Tris-HCl buffered aqueous solution described in step (2) was 8.5.
Furthermore, the mass ratio of the dopamine hydrochloride to the NixCoyS material in the step (2) is 1: 1-2.
Further, the drying temperature in the step (1) and the drying temperature in the step (2) are both 60 ℃.
Further, step (ii)(3) The calcination temperature is 300-700 ℃, the annealing time is 2-6 h, and the heating rate is 5 ℃ min -1 。
The carbon-coated cobalt-nickel binary transition metal sulfide NixCoyS @ C material prepared by the preparation method is used for a lithium ion battery cathode material.
Furthermore, the invention also provides a lithium ion battery cathode material of the carbon-coated bimetallic sulfide, and raw materials required in the preparation process are all of analytical grade, and further purification is not required.
Compared with the prior art, the invention has the following advantages:
the invention relates to a carbon-coated bimetallic sulfide lithium ion battery cathode material and a preparation method thereof, which have the advantages of simple preparation method and convenience for large-scale application. According to the method, nickel element is successfully introduced through a solvothermal reaction to prepare the bimetallic sulfide, and the electrochemical performance of the material is improved by utilizing the synergistic effect of the nickel element and the bimetallic sulfide; in addition, the carbon-coated bimetallic sulfide material is successfully obtained by coating polydopamine and calcining in an inert atmosphere. The coating of the carbon material not only further relieves the volume expansion problem of sulfide in the circulation process, but also enhances the conductivity of the negative electrode material. In conclusion, the invention provides a high-performance lithium ion battery cathode material.
Drawings
FIG. 1 is an XRD pattern of a NixCoyS @ C material prepared in example 1 of the present invention;
FIG. 2 is an SEM image of a NixCoyS @ C material prepared in example 1 of the present invention;
FIG. 3 shows that the NixCoyS @ C material prepared in example 1 is applied to a negative electrode material of a lithium ion battery at a current density of 200mA · g -1 The cycle performance curve of (a);
fig. 4 is a rate performance curve of the NixCoyS @ C material prepared in example 1 of the present invention applied to a negative electrode material of a lithium ion battery.
Detailed Description
The technical solutions of the present invention are further described in detail with reference to the drawings and the following specific embodiments, which are provided for illustration only and are not intended to limit the scope of the present invention.
Example 1
A preparation method of a carbon-coated cobalt-nickel binary transition metal sulfide negative electrode material comprises the following steps:
preparation of NixCoyS:
ultrasonically dispersing 0.582g of cobalt nitrate hexahydrate and 0.291g of nickel nitrate hexahydrate in 60mL of deionized water for 5min, then adding 0.3g of urea, magnetically stirring at 800rpm/min for 5min, then adding 0.386g of thiourea, stirring and ultrasonically dissolving to make the solution uniform, finally putting the mixture into an oven for reaction at the reaction temperature of 180 ℃ for 12h, and collecting a precipitated product after the reaction is finished. Repeatedly washing the product with deionized water, and drying in a 60 ℃ oven;
preparation of NixCoyS @ PDA:
dispersing 200mg of the obtained NixCoyS material in 100mL of Tris-HCl aqueous solution (pH 8.5), slowly adding 100mg of dopamine hydrochloride after magnetic stirring for 12 hours, then collecting the precipitated product, repeatedly washing the product with deionized water, and then drying in an oven at 60 ℃;
synthesis of NixCoyS @ C:
the obtained NixCoyS @ PDA is placed in a porcelain boat after being fully ground, and is put at 5 ℃ for min under the protection of argon -1 The temperature is raised to 500 ℃ at the heating rate, the temperature is kept for 3h, after the annealing treatment is finished, the sample is taken out under the protection of inert gas after being naturally cooled, and the NixCoyS @ C composite material is obtained, and the structural formula of the composite material is Ni0.48Co0.77S @ C determined through XRD phase analysis.
Example 2
A preparation method of a carbon-coated cobalt-nickel binary transition metal sulfide negative electrode material comprises the following steps:
preparation of NixCoyS:
ultrasonically dispersing 0.582g of cobalt nitrate hexahydrate and 0.291g of nickel nitrate hexahydrate in 60mL of deionized water for 5min, then adding 0.3g of urea, magnetically stirring at 800rpm/min for 5min, then adding 0.386g of thiourea, stirring and ultrasonically dissolving to make the mixture uniform, finally putting the mixture into an oven for reaction at the reaction temperature of 180 ℃ for 18h, collecting a precipitated product after the reaction is finished, repeatedly washing the product with deionized water, and then putting the product into the oven at the temperature of 60 ℃ for drying;
preparation of NixCoyS @ PDA:
dispersing 200mg of the obtained NixCoyS material in 100mL of Tris-HCl aqueous solution (pH 8.5), slowly adding 100mg of dopamine hydrochloride after magnetic stirring for 12 hours, then collecting the precipitated product, repeatedly washing the product with deionized water, and then drying in an oven at 60 ℃;
synthesis of NixCoyS @ C:
the obtained NixCoyS @ PDA is placed in a porcelain boat after being fully ground, and is put at 5 ℃ for min under the protection of argon -1 Heating to 500 ℃ at a heating rate, preserving heat for 3 hours, and taking out the sample after annealing treatment under the protection of inert gas after the sample is naturally cooled to obtain the NixCoyS @ C composite material;
example 3
A preparation method of a carbon-coated cobalt-nickel binary transition metal sulfide negative electrode material comprises the following steps:
preparation of NixCoyS:
ultrasonically dispersing 0.582g of cobalt nitrate hexahydrate and 0.291g of nickel nitrate hexahydrate in 60mL of deionized water for 5min, then adding 0.3g of urea, magnetically stirring at 800rpm/min for 5min, then adding 0.386g of thiourea, stirring and ultrasonically dissolving to make the mixture uniform, finally putting the mixture into an oven for reaction at the reaction temperature of 180 ℃ for 24h, collecting a precipitated product after the reaction is finished, repeatedly washing the product with deionized water, and then putting the product into the oven at the temperature of 60 ℃ for drying;
preparation of NixCoyS @ PDA:
200mg of the resulting NixCoyS material was dispersed in 100mL of an aqueous Tris-HCl solution (pH 8.5). Slowly adding 100mg of dopamine hydrochloride after magnetic stirring for 12 hours, then collecting a precipitate, repeatedly washing the precipitate with deionized water, and then drying the precipitate in a 60 ℃ oven;
synthesis of NixCoyS @ C:
the obtained NixCoyS @ PDA is placed in a porcelain boat after being fully ground, and is put at 5 ℃ for min under the protection of argon -1 Heating to 500 ℃ at a heating rate, preserving heat for 3 hours, and taking out the sample after annealing treatment under the protection of inert gas after the sample is naturally cooled to obtain the NixCoyS @ C composite material;
example 4
Taking the carbon-coated bimetallic sulfide lithium ion battery negative electrode material (hereinafter referred to as NixCoyS @ C) prepared in example 1 as a sample, an electrochemical performance test is carried out, and the specific method comprises the following steps:
uniformly mixing the NixCoyS @ C composite material, the Ketjen black and the binder (PVDF) in a ratio of 70mg to 20mg to 10mg, adding a solvent (NMP) to prepare slurry, coating the slurry on a copper foil, and drying at 60 ℃ for 12h to obtain the NixCoyS @ C negative plate. And then the lithium sheet and a button cell are assembled to carry out electrochemical performance test.
By aiming at the NixCoyS @ C composite material, the current density is 200 mA.g -1 The cycle performance test shows that the first discharge specific capacity of the NixCoyS @ C composite material is 1442.6 mAh.g -1 The charging specific capacity is 673.7mAh g -1 And the reversible specific capacity is still 834mAh g after circulating for 100 circles -1 And excellent cycle performance is shown.
The rate capability of the NixCoyS @ C composite material is tested and shown in FIG. 4. Through 5A. g -1 And 10A. g -1 After the high current is circulated, when the current density is restored to 100mA g -1 The charging specific capacity is recovered to 762.2mAh g -1 (initial Current Density of 100 mA. g) -1 The specific charging capacity is 851.6mAh g -1 ) And then still slowly increases. Therefore, the NixCoyS @ C composite material prepared by the embodiment has high cycle stability.
The above description is only a preferred embodiment of the present invention, and is not intended to limit the present invention in any way. Any modification, equivalent replacement, improvement and the like made within the technical scheme of the invention shall be included in the protection scope of the invention.
Claims (7)
1. A preparation method of a carbon-coated cobalt-nickel binary transition metal sulfide negative electrode material is characterized by comprising the following steps:
(1) preparation of NixCoyS:
mixing nickel nitrate hexahydrate, cobalt nitrate hexahydrate, urea and thiourea according to a molar ratio of 1:2: 2-8: 4-10, adding 60mL of deionized water, ultrasonically stirring until the solution is uniform, placing the solution in an oven for heating reaction to obtain a black precipitate, performing suction filtration to collect a product, repeatedly washing the product with deionized water, and placing the product in the oven for drying to obtain a NixCoyS material;
(2) synthesis of NixCoyS @ PDA:
dispersing the NixCoyS material obtained in the step (1) in 100mL of Tris-HCl buffer aqueous solution, adding dopamine hydrochloride after stirring and mixing uniformly, then washing and collecting a precipitate product, repeatedly washing the product with deionized water, and then placing the product in a drying oven for drying to obtain a NixCoyS @ PDA product;
(3) synthesis of NixCoyS @ C:
and (3) placing the NixCoyS @ PDA precursor obtained in the step (2) into a tubular furnace for calcining, and cooling to room temperature to obtain the NixCoyS @ C negative electrode material.
2. The method for preparing the carbon-coated cobalt-nickel binary transition metal sulfide negative electrode material as claimed in claim 1, wherein the reaction temperature in the step (1) is 180-200 ℃, and the reaction time is 12-24 hours.
3. The method for preparing a carbon-coated cobalt-nickel binary transition metal sulfide negative electrode material as claimed in claim 1, wherein the pH of the Tris-HCl buffered aqueous solution in the step (2) is 8.5.
4. The method for preparing the carbon-coated cobalt-nickel binary transition metal sulfide negative electrode material as claimed in claim 1, wherein the mass ratio of the dopamine hydrochloride to the NixCoyS material in the step (2) is 1: 1-2.
5. The method for preparing the carbon-coated cobalt-nickel binary transition metal sulfide negative electrode material as claimed in claim 1, wherein the drying temperature in the step (1) and the drying temperature in the step (2) are both 60 ℃.
6. The method for preparing the carbon-coated cobalt-nickel binary transition metal sulfide negative electrode material as claimed in claim 1, wherein the calcining temperature in the step (3) is 300-700 ℃, the annealing time is 2-6 h, and the heating rate is 5 ℃ per minute -1 。
7. The carbon-coated cobalt-nickel binary transition metal sulfide NixCoyS @ C material prepared by the preparation method of any one of claims 1-6 is used for a lithium ion battery cathode material.
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Cited By (1)
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