CN111675243B - Preparation method of zinc ferrite nanosheet negative electrode material, product and application - Google Patents

Preparation method of zinc ferrite nanosheet negative electrode material, product and application Download PDF

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CN111675243B
CN111675243B CN202010528467.9A CN202010528467A CN111675243B CN 111675243 B CN111675243 B CN 111675243B CN 202010528467 A CN202010528467 A CN 202010528467A CN 111675243 B CN111675243 B CN 111675243B
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CN111675243A (en
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崔大祥
吴晓燕
林琳
王敬锋
王岩岩
徐少洪
陈超
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Shanghai National Engineering Research Center for Nanotechnology Co Ltd
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    • C01—INORGANIC CHEMISTRY
    • C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G49/00—Compounds of iron
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    • H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
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    • H01—ELECTRIC ELEMENTS
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    • H01M4/485—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of mixed oxides or hydroxides for inserting or intercalating light metals, e.g. LiTi2O4 or LiTi2OxFy
    • H—ELECTRICITY
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    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
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    • H01M4/525—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of nickel, cobalt or iron of mixed oxides or hydroxides containing iron, cobalt or nickel for inserting or intercalating light metals, e.g. LiNiO2, LiCoO2 or LiCoOxFy
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Abstract

The invention provides a preparation method of a zinc ferrite nanosheet cathode material, a product and an application thereof. The first discharge specific capacity is 1580 mAh/g under the condition of 800 mA/g current density, the discharge specific capacity is relatively stable after 10 times of circulation and is 591 mAh/g, and the discharge specific capacity is 397 mAh/g after 50 times of circulation. The preparation process is relatively simple, the reaction is thorough, and the operation is easy.

Description

Preparation method, product and application of zinc ferrite nanosheet negative electrode material
Technical Field
The invention relates to a preparation method of a lithium battery negative electrode material, in particular to a preparation method of a zinc ferrite nanosheet negative electrode material, a product and an application thereof.
Background
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. At present, metal oxides and alloys with higher specific capacity become a new generation of electrode materials.
Zinc ferrite is a spinel-structured composite oxide, can be used as a lithium ion battery cathode material at present, and has high Li content through conversion and alloying reactions+A storage capacity. The material is considered to be a promising lithium ion battery cathode material.
The zinc ferrite theoretical specific capacity exceeds 1000 mAh/g, and the material has the advantages of wide raw materials and low production cost, and is an ideal lithium ion battery cathode material. However, during the charge and discharge cycle of zinc ferrite, the volume expansion and contraction cause the internal stress concentration of the electrode material, which causes electrode pulverization and reduces the cycle life. In order to improve the electrochemical performance of zinc ferrite, researchers have conducted a great deal of research, mainly on changing the structure and morphology of materials, doping, preparing composite materials and the like.
The invention provides a preparation method of a zinc ferrite nanosheet cathode material, which is characterized in that ferric salt is oxidized into ferrate by utilizing the strong oxidizing property of sodium peroxide, and then the zinc ferrite nanosheet is prepared through hydrothermal reduction, wherein the nanosheet is in a shape with a large specific surface area, can fully react with an electrolyte in the charging and discharging process, and is further favorable for improving the electrochemical performance of the material. The preparation process is relatively simple, the reaction is thorough, and the operation is easy.
Disclosure of Invention
In order to overcome the defect of poor electrochemical performance caused by volume expansion or pulverization of zinc ferrite in the charging and discharging processes, the invention aims to provide a preparation method of a zinc ferrite nanosheet negative electrode material.
Yet another object of the present invention is to: provides a zinc ferrite nanosheet 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 zinc ferrite nanosheet negative electrode material is characterized in that ferric salt is oxidized into ferrate by utilizing the strong oxidizing property of sodium peroxide, and then the zinc ferrite nanosheet is prepared through hydrothermal reduction, wherein the method comprises the following specific steps:
(1) Mixing 1.17 gNa2O2And 0.76 g FeSO4Mixing the materials evenly in a closed and dry environment, heating the mixture to 550 to 700 ℃ in an inert airflow, and reacting for 1 to 3 hours to obtain a product A containing 0.83 g of sodium ferrate;
(2) Dissolving a product A containing 0.83 g of sodium ferrate and soluble zinc salt in 80 mL of deionized water, and magnetically stirring until the mixture is uniform, wherein the mass ratio of iron to zinc is 2:1; then adding 2 to 4g of weak reducing agent and 3 to 5g of polyvinylpyrrolidone, magnetically stirring until the materials are uniformly dissolved, then transferring the materials into a reaction kettle, and reacting for 8 to 12 hours at 190 to 220 ℃; naturally cooling, centrifuging the obtained product, washing with deionized water and ethanol for 2 to 3 times respectively, and finally drying in vacuum overnight at 60 to 80 ℃ to obtain the final product.
Preferably, the zinc salt is one or a combination of zinc nitrate hexahydrate and zinc acetate dihydrate.
Preferably, the weak reducing agent is one or a combination of ascorbic acid and citric acid.
The invention provides a zinc ferrite nanosheet negative electrode material prepared according to any one of the methods.
The invention provides an application of a zinc ferrite nanosheet negative electrode material as a negative electrode material of a lithium ion battery.
According to the invention, ferric salt is oxidized into ferrate by utilizing the strong oxidizing property of sodium peroxide, and then zinc ferrite nanosheets are prepared by hydrothermal reduction, wherein the nanosheets have large specific surface areas, can fully react with electrolyte in the charging and discharging processes, and are further beneficial to improving the electrochemical performance of the material. The first discharge specific capacity is 1580 mAh/g under the condition of 800 mA/g current density, the discharge specific capacity is relatively stable after 10 times of circulation and is 591 mAh/g, and the discharge specific capacity is 397 mAh/g after 50 times of circulation. The preparation process is relatively simple, complete in reaction and easy to operate.
Drawings
FIG. 1 is a cycle life diagram of a zinc ferrite nanosheet negative electrode material of example 1;
FIG. 2 is a graph of the first charge-discharge performance of the zinc ferrite nanosheet negative electrode material of example 2;
fig. 3 is a graph of the first charge and discharge performance of the zinc ferrite nanosheet negative electrode material of example 3.
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 zinc ferrite nanosheet negative electrode material is prepared by oxidizing iron salt into ferrate by utilizing the strong oxidizing property of sodium peroxide, then preparing the zinc ferrite nanosheet through hydrothermal reduction, and comprising the following steps:
(1) Mixing 1.17 gNa2O2And 0.76 g FeSO4Mixing evenly in a closed and dry environment, heating to 600 ℃ in an inert gas flow, and reacting for 2 hours to obtain a product A containing 0.83 g of sodium ferrate;
(2) Dissolving a product A containing 0.83 g of sodium ferrate and 0.74 g of zinc nitrate hexahydrate in 80 mL of deionized water, and stirring uniformly by magnetic force, wherein the mass ratio of iron to zinc is 2:1; then 2g of weak reducing agent ascorbic acid and 3g of polyvinylpyrrolidone are added, the mixture is stirred by magnetic force until the mixture is dissolved evenly, and then the mixture is transferred into a reaction kettle to react for 10 hours at 200 ℃; naturally cooling, centrifuging the obtained product, washing with deionized water and ethanol for 3 times respectively, and finally drying at 80 ℃ in vacuum overnight to obtain the final product.
FIG. 1 is a cycle life diagram of a zinc ferrite nano flower-shaped negative electrode material under the current density of 800 mA/g, the first discharge specific capacity is 1580 mAh/g, the discharge specific capacity is relatively stable after 10 cycles, namely 591 mAh/g, and the discharge specific capacity is 397 mAh/g after 50 cycles.
Example 2
Similar to the embodiment 1, the zinc ferrite nanosheet negative electrode material is prepared by the following steps:
(1) Mixing 1.17 gNa2O2And 0.76 g FeSO4Mixing uniformly in a closed and dry environment, heating to 700 ℃ in an inert gas flow, and reacting for 1h to obtain a product A containing 0.83 g of sodium ferrate;
(2) Dissolving a product A containing 0.83 g of sodium ferrate and 0.55g of zinc acetate dihydrate into 80 mL of deionized water, and magnetically stirring until the mixture is uniform, wherein the mass ratio of iron to zinc is 2:1; then adding 4g of weak reducing agent citric acid and 5g of polyvinylpyrrolidone, magnetically stirring until the citric acid and the polyvinylpyrrolidone are uniformly dissolved, then transferring the mixture into a reaction kettle, and reacting for 8 hours at 220 ℃; naturally cooling, centrifuging the obtained product, washing with deionized water and ethanol for 3 times respectively, and finally drying at 80 ℃ in vacuum overnight to obtain the final product.
FIG. 2 is a diagram of the first charge and discharge performance of the zinc ferrite nano flower-shaped negative electrode material at a current density of 800 mA/g, the first discharge specific capacity is 1360 mAh/g, and the first charge specific capacity is 806 mAh/g.
Example 3
Similar to example 1, the zinc ferrite nanosheet negative electrode material is prepared by the following steps:
(1) 1.17 gNa2O2And 0.76 g FeSO4Mixing uniformly in a closed and dry environment, heating to 700 ℃ in an inert gas flow, and reacting for 1h to obtain a product A containing 0.83 g of sodium ferrate;
(2) Dissolving a product A containing 0.83 g of sodium ferrate and 0.74 g of zinc nitrate hexahydrate in 80 mL of deionized water, and magnetically stirring until the mixture is uniform, wherein the mass ratio of iron to zinc is 2:1; then adding 4g of weak reducing agent citric acid and 5g of polyvinylpyrrolidone, magnetically stirring until the citric acid and the polyvinylpyrrolidone are uniformly dissolved, then transferring the mixture into a reaction kettle, and reacting for 8 hours at 210 ℃; naturally cooling, centrifuging the obtained product, washing with deionized water and ethanol for 3 times respectively, and finally drying at 80 ℃ in vacuum overnight to obtain the final product.
FIG. 3 is a diagram of the first charge and discharge performance of the zinc ferrite nano flower-shaped negative electrode material at a current density of 800 mA/g, wherein the first discharge specific capacity is 1490 mAh/g, and the first charge specific capacity is 870 mAh/g.

Claims (4)

1. A preparation method of a zinc ferrite nanosheet cathode material is characterized in that ferric salt is oxidized into ferrate by utilizing the strong oxidizing property of sodium peroxide, and then the zinc ferrite nanosheet is prepared through hydrothermal reduction, and comprises the following steps:
(1) Mixing 1.17 gNa2O2And 0.76 g FeSO4Uniformly mixing the materials in a closed and dry environment, heating the mixture to 550 to 700 ℃ in an inert airflow, and reacting for 1 to 3 hours to obtain a product A containing 0.83 g of sodium ferrate;
(2) Dissolving a product A containing 0.83 g of sodium ferrate and soluble zinc salt in 80 mL of deionized water, and magnetically stirring until the mixture is uniform, wherein the mass ratio of iron to zinc is 2:1; then adding 2-4 g of weak reducing agent and 3-5 g of polyvinylpyrrolidone, magnetically stirring until the materials are uniformly dissolved, then transferring the materials into a reaction kettle, and reacting for 8-12 h at 190-220 ℃; naturally cooling, centrifuging the obtained product, washing with deionized water and ethanol for 2-3 times respectively, and finally drying in vacuum overnight at 60-80 ℃ to obtain a final product; wherein the content of the first and second substances,
the zinc salt is one or the combination of zinc nitrate hexahydrate and zinc acetate dihydrate;
the weak reducing agent is one or the combination of ascorbic acid or citric acid.
2. The preparation method of the zinc ferrite nanosheet negative electrode material according to claim 1, wherein the preparation method comprises the following steps:
(1) Mixing 1.17 gNa2O2And 0.76 g FeSO4Uniformly mixing in a closed and dry environment, heating to 600 ℃ in inert gas flow, and reacting for 2 hours to obtain a product A containing 0.83 g of sodium ferrate;
(2) Dissolving a product A containing 0.83 g of sodium ferrate and 0.74 g of zinc nitrate hexahydrate in 80 mL of deionized water, and stirring uniformly by magnetic force, wherein the mass ratio of iron to zinc is 2:1; then adding 2g of weak reducing agent ascorbic acid and 3g of polyvinylpyrrolidone, magnetically stirring until the ascorbic acid and the polyvinylpyrrolidone are uniformly dissolved, then transferring the mixture into a reaction kettle, and reacting for 10 hours at 200 ℃; naturally cooling, centrifuging the obtained product, washing with deionized water and ethanol for 3 times respectively, and finally drying at 80 ℃ in vacuum overnight to obtain the final product.
3. The preparation method of the zinc ferrite nanosheet negative electrode material according to claim 1, wherein the preparation method comprises the following steps:
(1) Mixing 1.17 gNa2O2And 0.76 g FeSO4Uniformly mixing the mixture in a closed and dry environment, heating the mixture to 700 ℃ in inert gas flow, and reacting the mixture for 1 hour to obtain a product A containing 0.83 g of sodium ferrate;
(2) Dissolving a product A containing 0.83 g of sodium ferrate and 0.55g of zinc acetate dihydrate into 80 mL of deionized water, and stirring uniformly by magnetic force, wherein the mass ratio of iron to zinc is 2:1; then adding 4g of weak reducing agent citric acid and 5g of polyvinylpyrrolidone, magnetically stirring until the citric acid and the polyvinylpyrrolidone are uniformly dissolved, then transferring the mixture into a reaction kettle, and reacting for 8 hours at 220 ℃; naturally cooling, centrifuging the obtained product, washing with deionized water and ethanol for 3 times respectively, and finally drying at 80 ℃ in vacuum overnight to obtain the final product.
4. The preparation method of the zinc ferrite nanosheet negative electrode material according to claim 1, characterized by being prepared by the steps of:
(1) Mixing 1.17 gNa2O2And 0.76 g FeSO4Uniformly mixing the mixture in a closed and dry environment, heating the mixture to 700 ℃ in inert gas flow, and reacting the mixture for 1 hour to obtain a product A containing 0.83 g of sodium ferrate;
(2) Dissolving a product A containing 0.83 g of sodium ferrate and 0.74 g of zinc nitrate hexahydrate in 80 mL of deionized water, and stirring uniformly by magnetic force, wherein the mass ratio of iron to zinc is 2:1; then adding 4g of weak reducing agent citric acid and 5g of polyvinylpyrrolidone, magnetically stirring until the citric acid and the polyvinylpyrrolidone are uniformly dissolved, then transferring the mixture into a reaction kettle, and reacting for 8 hours at 210 ℃; naturally cooling, centrifuging the obtained product, washing with deionized water and ethanol for 3 times respectively, and finally drying at 80 ℃ in vacuum overnight to obtain the final product.
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