CN110156079B - Preparation method of linear copper vanadate negative electrode material, product and application - Google Patents

Preparation method of linear copper vanadate negative electrode material, product and application Download PDF

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CN110156079B
CN110156079B CN201910473985.2A CN201910473985A CN110156079B CN 110156079 B CN110156079 B CN 110156079B CN 201910473985 A CN201910473985 A CN 201910473985A CN 110156079 B CN110156079 B CN 110156079B
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copper
copper foil
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metavanadate
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CN110156079A (en
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何丹农
吴晓燕
林琳
陈振
王敬锋
徐少洪
陈超
金彩虹
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Shanghai National Engineering Research Center for Nanotechnology Co Ltd
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Abstract

The invention provides a preparation method of a linear copper vanadate negative electrode material, which is characterized in that copper foil is used as a copper source, a hydrothermal method is used for preparing nano linear copper vanadate, and the material has larger specific surface area and conductivity and is further favorable for improving the electrochemical performance of the material. The first discharge specific capacity is 1500 mAh/g, and the specific capacity is 302 mAh/g after 50 times of circulation. Compared with common composite oxides, the cycle life is relatively stable. The preparation process is relatively simple and easy to operate.

Description

Preparation method of linear copper vanadate negative electrode material, product and application
Technical Field
The invention relates to a preparation method of a lithium battery cathode material, in particular to a preparation method of a linear copper vanadate cathode material, and a product and application thereof.
Background
With the development of society, lithium ion batteries are receiving much attention. The lithium ion battery is the most ideal rechargeable battery in the world at present, and has the advantages of high energy density, long cycle life, no memory effect, small pollution and the like. With the progress of technology, lithium ion batteries are widely applied to the fields of electric automobiles, aerospace, biomedicine and the like, so that the research and development of lithium ion batteries for power and related materials have great significance. For power lithium ion batteries, the key is to increase the power density and energy density, and the improvement of the power density and energy density is fundamentally the improvement of electrode materials, particularly negative electrode materials.
Since the early 90 s of the last century, the japanese scientists developed carbon materials with layered structures, which were the first materials studied by people and applied to the commercialization of lithium ion batteries, and still remain one of the major points of attention and research, but carbon negative electrode materials have some defects: when the battery is formed, the electrolyte reacts with the electrolyte to form an SEI film, so that the electrolyte is consumed and the first coulombic efficiency is low; when the battery is overcharged, metal lithium may be precipitated on the surface of the carbon electrode to form lithium dendrite to cause short circuit, so that the temperature is increased and the battery explodes; in addition, the diffusion coefficient of lithium ions in the carbon material is small, so that the battery cannot realize large-current charging and discharging, and the application range of the lithium ion battery is limited.
Copper vanadate (Cu)3V2O8) Is a spinel-structured composite oxide, can be used as a lithium ion battery cathode material at present, and has higher Li content through conversion and alloying reactions+A storage capacity. The material is considered to be a promising lithium ion battery cathode material.
The invention provides a preparation method of a linear copper vanadate negative electrode material, which is characterized in that copper foil is used as a copper source, a hydrothermal method is used for preparing nano linear copper vanadate, and the material has larger specific surface area and conductivity and is further favorable for improving the electrochemical performance of the material. The preparation process is relatively simple and easy to operate.
Disclosure of Invention
In order to overcome the defect of poor electrochemical performance of copper vanadate, the invention aims to provide a preparation method of a linear copper vanadate negative electrode material.
Yet another object of the present invention is to: provides a linear copper vanadate negative electrode material product obtained by the method.
Yet another object of the present invention is to: provides an application of the product.
The purpose of the invention is realized by the following scheme: a preparation method of a linear copper vanadate negative electrode material is characterized in that copper foil is used as a copper source, and nano linear copper vanadate is prepared from a substrate by a hydrothermal method, and the method comprises the following specific steps:
(1) shearing 0.1-0.2 mmol of 1 cm multiplied by 1 cm copper foil, cleaning, drying and placing at the bottom of a 100 mL reaction kettle;
(2) mixing metavanadate, urea, an ammonium fluoride solution and hydrogen peroxide, and adding the mixture into a reaction kettle, wherein the molar ratio of the reacted copper foil, the metavanadate, the urea and the ammonium fluoride is 0.009 mmol: 0.006 mmol: 0.016 mmol: 0.04 mmol, magnetically stirring for 15-30 min at normal temperature, transferring into a hydrothermal reaction kettle, and reacting for 3-5 h at 130-150 ℃;
(3) cooling to room temperature, carrying out vacuum filtration on the precipitate, washing with water and ethanol for several times, and drying in a vacuum oven at 60-80 ℃ for 10-15 h;
(4) calcining the precipitate at 500-700 ℃ for 3-5 h to obtain a linear copper vanadate material.
The metavanadate is one or the combination of ammonium metavanadate and copper metavanadate.
The mass percentage of the hydrogen peroxide is 10-30%.
The invention provides a linear copper vanadate anode material prepared by any one of the methods.
The invention provides an application of a linear copper vanadate negative electrode material as a negative electrode material in a lithium ion battery.
Has the advantages that:
the invention provides a preparation method of a linear copper vanadate negative electrode material, which is characterized in that copper foil is used as a copper source, a hydrothermal method is used for preparing nano linear copper vanadate, and the material has larger specific surface area and conductivity and is further favorable for improving the electrochemical performance of the material. The first discharge specific capacity is 1500 mAh/g, and the specific capacity is 302 mAh/g after 50 times of circulation. Compared with common composite oxides, the cycle life is relatively stable. The preparation process is relatively simple and easy to operate.
Drawings
FIG. 1 shows Cu of example 13V2O8SEM picture of (1);
FIG. 2 is Cu of example 23V2O8A cycle life map of;
FIG. 3 is example 3Cu3V2O8The rate performance graph of (1).
Detailed Description
The present invention is described in detail by the following specific examples, but the scope of the present invention is not limited to these examples.
Example 1
A linear copper vanadate negative electrode material is prepared from copper foil serving as a copper source and a substrate by a hydrothermal method, and comprises the following specific steps:
(1) shearing a copper foil with the thickness of 1 cm multiplied by 1 cm of 0.1 mmol, cleaning and drying the copper foil, and placing the copper foil at the bottom of a 100 mL reaction kettle;
(2) mixing ammonium metavanadate, urea, an ammonium fluoride solution and hydrogen peroxide, and adding into a reaction kettle, wherein the molar ratio of the reacted copper foil, ammonium metavanadate, urea and ammonium fluoride is 0.009 mmol: 0.006 mmol: 0.016 mmol: 0.04 mmol and 10 percent of hydrogen peroxide by mass percent, magnetically stirring for 15 min at normal temperature, transferring into a hydrothermal reaction kettle, and reacting for 5 h at 130 ℃;
(3) cooling to room temperature, carrying out vacuum filtration on the precipitate, washing with water and ethanol for several times, and drying in a vacuum oven at 80 ℃ for 10 h;
(4) and calcining the precipitate at 500 ℃ for 5 hours to obtain a linear copper vanadate material. FIG. 1 is Cu3V2O8The SEM image shows that the material is a nanowire consisting of nano particles, has a large specific surface area and is beneficial to improving the electrochemical performance of the material.
Example 2
A linear copper vanadate anode material is prepared by the following specific steps:
(1) shearing a copper foil with the thickness of 1 cm multiplied by 1 cm of 0.1 mmol, cleaning and drying the copper foil, and placing the copper foil at the bottom of a 100 mL reaction kettle;
(2) mixing and adding a solution of copper metavanadate, urea, ammonium fluoride and hydrogen peroxide into a reaction kettle, wherein the molar ratio of the reacted copper foil to the reacted copper metavanadate to the reacted urea to the reacted ammonium fluoride is 0.009 mmol: 0.006 mmol: 0.016 mmol: 0.04 mmol, 20% hydrogen peroxide by mass, magnetically stirring for 30 min at normal temperature, transferring into a hydrothermal reaction kettle, and reacting for 3 h at 150 ℃;
(3) cooling to room temperature, carrying out vacuum filtration on the precipitate, washing with water and ethanol for several times, and drying in a vacuum oven at 60 ℃ for 15 h;
(4) and calcining the precipitate at 600 ℃ for 5 hours to obtain a linear copper vanadate material.
FIG. 2 is Cu3V2O8A cycle life map of; the first discharge specific capacity is 1500 mAh/g, and the specific capacity is 302 mAh/g after 50 times of circulation. Compared with common composite oxides, the cycle life is relatively stable.
Example 3
A linear copper vanadate anode material is prepared by the following specific steps:
(1) shearing 0.2 mmol of copper foil with the thickness of 1 cm multiplied by 1 cm, cleaning and drying the copper foil, and then placing the copper foil at the bottom of a 100 mL reaction kettle;
(2) mixing and adding a solution of copper metavanadate, urea, ammonium fluoride and hydrogen peroxide into a reaction kettle, wherein the molar ratio of the reacted copper foil to the reacted copper metavanadate to the reacted urea to the reacted ammonium fluoride is 0.009 mmol: 0.006 mmol: 0.016 mmol: 0.04 mmol, 30% hydrogen peroxide by mass, magnetically stirring for 30 min at normal temperature, transferring into a hydrothermal reaction kettle, and reacting for 3 h at 150 ℃;
(3) cooling to room temperature, carrying out vacuum filtration on the precipitate, washing with water and ethanol for several times, and drying in a vacuum oven at 60 ℃ for 15 h;
(4) and calcining the precipitate at 700 ℃ for 5 h to obtain a linear copper vanadate material.
FIG. 3 shows Cu of this example3V2O8The average specific discharge capacity is 780 mAh/g under the current density of 100 mA/g, the average specific discharge capacity is 490 mAh/g under the current density of 200 mA/g and the average specific discharge capacity is 400 mA/gThe capacity is about 390 mAh/g, the average specific discharge capacity is about 300 mAh/g under the current density condition of 800 mA/g, the average specific discharge capacity is about 190 mAh/g under the current density condition of 1600 mA/g, and the average specific discharge capacity is about 170 mAh/g under the current density condition of 2000 mA/g. Under the condition of large current density, the specific capacity is relatively high.

Claims (6)

1. A preparation method of a linear copper vanadate negative electrode material is characterized in that copper foil is used as a copper source, and nano linear copper vanadate is prepared from a substrate by a hydrothermal method, and the method comprises the following specific steps:
(1) shearing 0.1-0.2 mmol of 1 cm multiplied by 1 cm copper foil, cleaning, drying and placing at the bottom of a 100 mL reaction kettle;
(2) mixing metavanadate, urea, an ammonium fluoride solution and hydrogen peroxide, and adding the mixture into a reaction kettle, wherein the molar ratio of the reacted copper foil, the metavanadate, the urea and the ammonium fluoride is 0.009 mmol: 0.006 mmol: 0.016 mmol: 0.04 mmol, magnetically stirring for 15-30 min at normal temperature, transferring into a hydrothermal reaction kettle, and reacting for 3-5 h at 130-150 ℃;
(3) cooling to room temperature, carrying out vacuum filtration on the precipitate, washing with water and ethanol for several times, and drying in a vacuum oven at 60-80 ℃ for 10-15 h;
(4) calcining the precipitate at 500-700 ℃ for 3-5 h to obtain a linear copper vanadate material.
2. The method according to claim 1, wherein the metavanadate is one or a combination of ammonium metavanadate and copper metavanadate.
3. The preparation method of the linear copper vanadate anode material according to claim 1, wherein the hydrogen peroxide is 10-30% by mass.
4. The method for preparing the linear copper vanadate anode material according to any one of claims 1 to 3, comprising the following steps:
(1) shearing a copper foil with the thickness of 1 cm multiplied by 1 cm of 0.1 mmol, cleaning and drying the copper foil, and placing the copper foil at the bottom of a 100 mL reaction kettle;
(2) mixing ammonium metavanadate, urea, an ammonium fluoride solution and hydrogen peroxide, and adding the mixture into a reaction kettle, wherein the molar ratio of the reacted copper foil to the ammonium metavanadate to the urea to the ammonium fluoride is 0.009 mmol: 0.006 mmol: 0.016 mmol: 0.04 mmol and 10 percent of hydrogen peroxide by mass percent, magnetically stirring for 15 min at normal temperature, transferring into a hydrothermal reaction kettle, and reacting for 5 h at 130 ℃;
(3) cooling to room temperature, carrying out vacuum filtration on the precipitate, washing with water and ethanol for several times, and drying in a vacuum oven at 80 ℃ for 10 h;
(4) and calcining the precipitate at 500 ℃ for 5 hours to obtain a linear copper vanadate material.
5. The method for preparing the linear copper vanadate anode material according to any one of claims 1 to 3, comprising the following steps:
(1) shearing a copper foil with the thickness of 1 cm multiplied by 1 cm of 0.1 mmol, cleaning and drying the copper foil, and placing the copper foil at the bottom of a 100 mL reaction kettle;
(2) mixing and adding a solution of copper metavanadate, urea, ammonium fluoride and hydrogen peroxide into a reaction kettle, wherein the molar ratio of the reacted copper foil to the reacted copper metavanadate to the reacted urea to the reacted ammonium fluoride is 0.009 mmol: 0.006 mmol: 0.016 mmol: 0.04 mmol, 20% hydrogen peroxide by mass, magnetically stirring for 30 min at normal temperature, transferring into a hydrothermal reaction kettle, and reacting for 3 h at 150 ℃;
(3) cooling to room temperature, carrying out vacuum filtration on the precipitate, washing with water and ethanol for several times, and drying in a vacuum oven at 60 ℃ for 15 h;
(4) and calcining the precipitate at 600 ℃ for 5 hours to obtain a linear copper vanadate material.
6. The method for preparing the linear copper vanadate anode material according to any one of claims 1 to 3, comprising the following steps:
(1) shearing 0.2 mmol of copper foil with the thickness of 1 cm multiplied by 1 cm, cleaning and drying the copper foil, and then placing the copper foil at the bottom of a 100 mL reaction kettle;
(2) mixing and adding a solution of copper metavanadate, urea, ammonium fluoride and hydrogen peroxide into a reaction kettle, wherein the molar ratio of the reacted copper foil to the reacted copper metavanadate to the reacted urea to the reacted ammonium fluoride is 0.009 mmol: 0.006 mmol: 0.016 mmol: 0.04 mmol, 30% hydrogen peroxide by mass, magnetically stirring for 30 min at normal temperature, transferring into a hydrothermal reaction kettle, and reacting for 3 h at 150 ℃;
(3) cooling to room temperature, carrying out vacuum filtration on the precipitate, washing with water and ethanol for several times, and drying in a vacuum oven at 60 ℃ for 15 h;
(4) and calcining the precipitate at 700 ℃ for 5 h to obtain a linear copper vanadate material.
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CN108075123A (en) * 2017-12-14 2018-05-25 陕西科技大学 A kind of solvent-thermal method prepares flower-shaped Cu2V2O7The method of-CuO nano-complexes
CN108117098A (en) * 2017-12-14 2018-06-05 陕西科技大学 A kind of coralliform α-Cu2V2O7Raw powder's production technology
CN108134058A (en) * 2017-12-14 2018-06-08 陕西科技大学 A kind of Cu5V2O10The preparation method of-CuO composite granules

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