CN114180537B - Preparation method of nitrogen-doped carbon-coated negative electrode material for lithium ion battery - Google Patents
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Abstract
The invention discloses a preparation method of a nitrogen-doped carbon-coated anode material for a lithium ion battery. The anode material obtained by the method contains MnSe-Fe 3 Se 4 The three-dimensional heterostructure can provide stable environment for lithium ion transmission, so that the material capacity is improved, the material expansion is inhibited, and the cycle life of the material is prolonged.
Description
Technical Field
The invention relates to a preparation method of a nitrogen-doped carbon-coated negative electrode material for a lithium ion battery, and belongs to the field of material preparation.
Background
In recent years, lithium ion batteries have been widely used as green clean new energy sources for energy storage and electric automobiles. Higher demands are placed on the development of lithium ion batteries, such as high capacity, high rate charge and discharge, long cycling, and the like. In order to improve the electrochemical performance of the lithium ion battery, a negative electrode material matched with the lithium ion battery is still to be further developed.
In recent years, prussian blue-derived nanomaterial is widely applied to the field of energy sources due to the special physical and chemical properties of the nanomaterial, and the nanomaterial comprises a lithium ion battery, a flow battery, a fuel battery, a sodium ion battery, a super capacitor, an electrocatalytic function and the like. Such materials have received extensive attention from researchers in the energy field due to their excellent properties in the energy storage field.
However, prussian blue derived materials also suffer from drawbacks such as high expansion rates and rapid capacity drops in the future. How to solve this drawback is therefore a limiting factor for the widespread use of such materials. This document aims at solving this problem by a series of modifications to the material.
Disclosure of Invention
The invention aims to provide a preparation method of a nitrogen-doped carbon-coated negative electrode material for a lithium ion battery.
The invention aims at realizing the following scheme: a preparation method of a nitrogen-doped carbon-coated negative electrode material for a lithium ion battery comprises the steps of complexing Prussian blue similar compound with manganese salt to form Mn-Fe-PBA microtubes, coating the surfaces of the microtubes by chitosan, and then obtaining a Mn Se-Fe-containing cathode material through mixing and calcining with selenium powder 3 Se 4 The three-dimensional heterostructure nitrogen-doped carbon-coated anode material comprises the following steps:
(1) Dissolving manganese salt in deionized water, and electromagnetically stirring for 10 minutes to form a solution A;
(2) Dissolving Prussian blue compounds and sodium citrate in deionized water, and carrying out electromagnetic stirring for 10 minutes to form a solution B, wherein the Prussian blue compounds are one or a combination of potassium ferrocyanide and sodium ferrocyanide;
(3) Slowly pouring the solution A into the solution B, continuously stirring to obtain a mixed solution, aging the mixed solution at room temperature for 24 hours, centrifugally collecting precipitate, washing with deionized water, and drying;
(4) Dispersing the precipitate obtained in the step (3) into Tris buffer solution, stirring and carrying out ultrasonic treatment for 20 minutes, adding chitosan, stirring at room temperature for 6 hours, centrifugally collecting a product, washing with deionized water and ethanol, and drying to obtain the product;
(5) Mixing the product of the step (4) with selenium powder according to a mass ratio of 1:2-1:3, fully mixing, calcining under protective atmosphere to obtain the MnSe-Fe-containing material 3 Se 4 Three-dimensional heterostructure nitrogen-doped carbon-coated anode materials.
Wherein the manganese salt in the step (1) is one or a combination of manganese chloride, manganese sulfate and manganese nitrate.
In the step (5), calcination is carried out at 400-600 ℃ for 2-4 hours, and the protective atmosphere can be argon.
The beneficial effects are that:
the invention provides a preparation method of a nitrogen-doped carbon-coated anode material for a lithium ion battery, and provides a preparation method of a novel anode material with simple preparation process, short flow and strong operability. Complexing Prussian blue compound with manganese salt to form Mn-Fe-PBA microtubule, coating the surface of the microtubule by chitosan, and mixing and calcining the microtubule with selenium powder to obtain the nitrogen-doped carbon-coated cathode material. The anode material obtained by the method contains MnSe-Fe 3 Se 4 The three-dimensional heterostructure can provide stable environment for lithium ion transmission, so that the material capacity is improved, the material expansion is inhibited, and the cycle life of the material is prolonged.
Drawings
FIG. 1 is a cycle chart of example 1.
Detailed Description
The present invention will be described in detail by way of specific examples, which are merely illustrative of the present invention, but the scope of the present invention is not limited to these examples.
Example 1:
a nitrogen-doped carbon-coated negative electrode material for lithium ion battery is prepared through complexing Prussian blue similar compound with Mn salt to form Mn-Fe-PBA microtube, coating the surface with chitosan, and calcining with Se powder to obtain MnSe-Fe 3 Se 4 The three-dimensional heterostructure nitrogen-doped carbon-coated anode material is prepared according to the following steps:
(1) 0.0938g of manganese salt is dissolved in 100ml of deionized water and is stirred electromagnetically for 10 minutes to form a solution A;
(2) Dissolving 0.038mg of potassium ferrocyanide and 0.56g of sodium citrate in deionized water, and carrying out electromagnetic stirring for 10 minutes to form a solution B, wherein the Prussian blue compound is one or a combination of potassium ferrocyanide and sodium ferrocyanide;
(3) Slowly pouring the solution A into the solution B, continuously stirring to obtain a mixed solution, aging the mixed solution at room temperature for 24 hours, centrifugally collecting precipitate, washing with deionized water, and drying;
(4) Dispersing 50mg of the precipitate obtained in the step (3) into 100ml of 15mM Tris buffer solution, stirring and carrying out ultrasonic treatment for 20 minutes, adding 25mg of chitosan, stirring at room temperature for 6 hours, centrifugally collecting a product, washing with deionized water and ethanol, and drying to obtain the product;
(5) Mixing the product of the step (4) with selenium powder according to a mass ratio of 1:2, fully mixing, calcining under argon atmosphere, calcining at 450 ℃ for 3 hours to obtain the alloy containing MnSe-Fe 3 Se 4 Three-dimensional heterostructure nitrogen-doped carbon-coated anode materials.
The obtained negative electrode powder was assembled into a button-type half cell for electrical property test, as shown in fig. 1. The graph shows that the battery capacity is high and can reach 1298mAh/g, the cycle performance is stable, the capacity attenuation after 100 circles of cycle is small, and the capacity retention rate can reach 92.6%.
Example 2:
a nitrogen-doped carbon-coated negative electrode material for a lithium ion battery is prepared by the following steps, similar to the steps of example 1:
(1) 0.0938g of manganese chloride is dissolved in 100ml of deionized water and is stirred electromagnetically for 10 minutes to form a solution A;
(2) Dissolving 0.031mg of sodium ferrocyanide and 0.56g of sodium citrate in deionized water, and performing electromagnetic stirring for 10 minutes to form a solution B;
(3) Slowly pouring the solution A into the solution B, continuously stirring to obtain a mixed solution, aging the mixed solution at room temperature for 24 hours, centrifuging to collect precipitate, washing with deionized water, and drying;
(4) Dispersing 50mg of the precipitate obtained in the step (3) into 100ml of 15mM Tris buffer solution, stirring and carrying out ultrasonic treatment for 20 minutes, adding 25mg of chitosan, stirring at room temperature for 6 hours, centrifugally collecting a product, washing with deionized water and ethanol, and drying;
(5) Mixing the product of the step (4) with selenium powder according to the weight ratio of 1:3, fully mixing, calcining under the protection of argon atmosphere, calcining at 500 ℃ for 2 hours to obtain the MnSe-Fe 3 Se 4 Three-dimensional heterostructure nitrogen-doped carbon-coated anode materials.
Example 3:
a nitrogen-doped carbon-coated negative electrode material for a lithium ion battery is prepared by the following steps, similar to the steps of example 1:
(1) 0.0938g of manganese chloride is dissolved in 100ml of deionized water and is stirred electromagnetically for 10 minutes to form a solution A;
(2) Dissolving 0.038g of potassium ferrocyanide and 0.56g of sodium citrate in deionized water, and carrying out electromagnetic stirring for 10 minutes to form a solution B;
(3) Slowly pouring the solution A into the solution B, continuously stirring to obtain a mixed solution, aging the mixed solution at room temperature for 24 hours, centrifuging to collect precipitate, washing with deionized water, and drying;
(4) Dispersing 50mg of the precipitate obtained in the step (3) into 100ml of 15mM Tris buffer solution, stirring and carrying out ultrasonic treatment for 20 minutes, then adding 25mg of chitosan, stirring at room temperature for 6 hours, centrifugally collecting a product, washing with deionized water and ethanol, and drying;
(5) Mixing the product of the step (4) with selenium powder according to the weight ratio of 1:2.5, calcining under the protection of argon atmosphere at 550 ℃ for 4 hours to obtain the MnSe-Fe 3 Se 4 Three-dimensionalHeterostructure nitrogen doped carbon coated negative electrode material.
Claims (6)
1. A preparation method of a nitrogen-doped carbon-coated anode material for a lithium ion battery is characterized in that a Prussian blue similar compound is complexed with manganese salt to form Mn-Fe-PBA microtubes, chitosan is adopted to coat the surfaces of the microtubes, and then the surface of the microtubes is mixed with selenium powder to obtain the anode material containing MnSe-Fe 3 Se 4 The three-dimensional heterostructure nitrogen-doped carbon-coated anode material comprises the following steps:
(1) Dissolving manganese salt in deionized water, and electromagnetically stirring for 10 minutes to form a solution A;
(2) Dissolving Prussian blue compounds and sodium citrate in deionized water, and carrying out electromagnetic stirring for 10 minutes to form a solution B, wherein the Prussian blue compounds are one or a combination of potassium ferrocyanide and sodium ferrocyanide;
(3) Slowly pouring the solution A into the solution B, continuously stirring to obtain a mixed solution, aging the mixed solution at room temperature for 24 hours, centrifugally collecting precipitate, washing with deionized water, and drying;
(4) Dispersing the precipitate obtained in the step (3) into Tris buffer solution, stirring and carrying out ultrasonic treatment for 20 minutes, adding chitosan, stirring at room temperature for 6 hours, centrifugally collecting a product, washing with deionized water and ethanol, and drying to obtain the product;
(5) Mixing the product of the step (4) with selenium powder according to a mass ratio of 1:2-1:3, fully mixing, calcining under protective atmosphere to obtain the MnSe-Fe-containing material 3 Se 4 Three-dimensional heterostructure nitrogen-doped carbon-coated anode materials.
2. The method for preparing a nitrogen-doped carbon-coated anode material for a lithium ion battery according to claim 1, wherein the manganese salt in the step (1) is one or a combination of manganese chloride, manganese sulfate and manganese nitrate.
3. The method for producing a nitrogen-doped carbon-coated negative electrode material for a lithium ion battery according to claim 1, wherein in the step (5), the calcination temperature is 400 to 600 ℃ and the holding time is 2 to 4 hours.
4. A method for producing a nitrogen-doped carbon-coated anode material for lithium ion batteries according to any one of claims 1 to 3, characterized by comprising the steps of:
(1) 0.0938g of manganese salt is dissolved in 100ml of deionized water and is stirred electromagnetically for 10 minutes to form a solution A;
(2) Dissolving 0.038mg of potassium ferrocyanide and 0.56g of sodium citrate in deionized water, and carrying out electromagnetic stirring for 10 minutes to form a solution B, wherein the Prussian blue compound is one or a combination of potassium ferrocyanide and sodium ferrocyanide;
(3) Slowly pouring the solution A into the solution B, continuously stirring to obtain a mixed solution, aging the mixed solution at room temperature for 24 hours, centrifugally collecting precipitate, washing with deionized water, and drying;
(4) Dispersing 50mg of the precipitate obtained in the step (3) into 100ml of 15mM Tris buffer solution, stirring and carrying out ultrasonic treatment for 20 minutes, adding 25mg of chitosan, stirring at room temperature for 6 hours, centrifugally collecting a product, washing with deionized water and ethanol, and drying to obtain the product;
(5) Mixing the product of the step (4) with selenium powder according to a mass ratio of 1:2, fully mixing, calcining under argon atmosphere, calcining at 450 ℃ for 3 hours to obtain the alloy containing MnSe-Fe 3 Se 4 Three-dimensional heterostructure nitrogen-doped carbon-coated anode materials.
5. A method for producing a nitrogen-doped carbon-coated anode material for lithium ion batteries according to any one of claims 1 to 3, characterized by comprising the steps of: (1) 0.0938g of manganese chloride is dissolved in 100ml of deionized water and is stirred electromagnetically for 10 minutes to form a solution A;
(2) Dissolving 0.031mg of sodium ferrocyanide and 0.56g of sodium citrate in deionized water, and performing electromagnetic stirring for 10 minutes to form a solution B;
(3) Slowly pouring the solution A into the solution B, continuously stirring to obtain a mixed solution, aging the mixed solution at room temperature for 24 hours, centrifuging to collect precipitate, washing with deionized water, and drying;
(4) Dispersing 50mg of the precipitate obtained in the step (3) into 100ml of 15mM Tris buffer solution, stirring and carrying out ultrasonic treatment for 20 minutes, adding 25mg of chitosan, stirring at room temperature for 6 hours, centrifugally collecting a product, washing with deionized water and ethanol, and drying;
(5) Mixing the product of the step (4) with selenium powder according to the weight ratio of 1:3, fully mixing, calcining under the protection of argon atmosphere, calcining at 500 ℃ for 2 hours to obtain the MnSe-Fe 3 Se 4 Three-dimensional heterostructure nitrogen-doped carbon-coated anode materials.
6. A method for producing a nitrogen-doped carbon-coated anode material for lithium ion batteries according to any one of claims 1 to 3, characterized by comprising the steps of: (1) 0.0938g of manganese chloride is dissolved in 100ml of deionized water and is stirred electromagnetically for 10 minutes to form a solution A;
(2) Dissolving 0.038g of potassium ferrocyanide and 0.56g of sodium citrate in deionized water, and carrying out electromagnetic stirring for 10 minutes to form a solution B;
(3) Slowly pouring the solution A into the solution B, continuously stirring to obtain a mixed solution, aging the mixed solution at room temperature for 24 hours, centrifuging to collect precipitate, washing with deionized water, and drying;
(4) Dispersing 50mg of the precipitate obtained in the step (3) into 100ml of 15mM Tris buffer solution, stirring and carrying out ultrasonic treatment for 20 minutes, then adding 25mg of chitosan, stirring at room temperature for 6 hours, centrifugally collecting a product, washing with deionized water and ethanol, and drying;
(5) Mixing the product of the step (4) with selenium powder according to the weight ratio of 1:2.5, calcining under the protection of argon atmosphere at 550 ℃ for 4 hours to obtain the MnSe-Fe 3 Se 4 Three-dimensional heterostructure nitrogen-doped carbon-coated anode materials.
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