CN110165173B - Preparation method of flexible transition metal sulfide negative electrode material of sodium ion battery - Google Patents
Preparation method of flexible transition metal sulfide negative electrode material of sodium ion battery Download PDFInfo
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- CN110165173B CN110165173B CN201910415365.3A CN201910415365A CN110165173B CN 110165173 B CN110165173 B CN 110165173B CN 201910415365 A CN201910415365 A CN 201910415365A CN 110165173 B CN110165173 B CN 110165173B
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- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/054—Accumulators with insertion or intercalation of metals other than lithium, e.g. with magnesium or aluminium
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- 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
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Abstract
The invention discloses a preparation method of a flexible transition metal sulfide negative electrode material of a sodium ion battery, which comprises the following steps: (1) weighing glucose, transition metal salt and thioacetamide, adding the glucose, the transition metal salt and the thioacetamide into a mixed solvent consisting of a water-soluble organic solvent and deionized water, and uniformly dispersing to obtain a solution with the mass fraction of 3% -10%; (2) soaking melamine sponge in the solution in the step (1), taking out, and drying in an oven for 12h to obtain a transition metal complex loaded by the melamine sponge; (3) and (3) placing the prepared melamine sponge-loaded transition metal complex in a tubular furnace, and carrying out heat treatment for 1-4 h to obtain the flexible transition metal sulfide negative electrode material. The preparation method is simple and easy for large-scale production, and the prepared flexible electrode does not need a binder, a conductive agent and a metal current collector, has excellent cycle stability and rate capability, and has wide application prospect in the field of flexible devices.
Description
Technical Field
The invention relates to preparation of a flexible negative electrode material of a battery, in particular to a preparation method of a flexible transition metal sulfide negative electrode material of a sodium-ion battery.
Background
Lithium ion batteries have been widely used in the field of energy storage in portable electronic devices, electric vehicles, and the like. However, the lithium resource is relatively deficient in nature, so that the manufacturing cost of the lithium ion battery is gradually increased, and the lithium ion battery is manufactured on a large scaleThe aspect of energy storage is limited. Because of abundant raw materials and low price, the sodium ion battery is considered as a new generation of energy storage device, and is expected to replace a lithium ion battery and widely applied to the fields of mobile electronic devices, large-scale energy storage equipment and the like. Due to Na+Radius ratio Li+Large, so the graphite anode materials widely used in lithium ion batteries are not suitable for sodium ion batteries. Therefore, the development of the sodium ion battery cathode material can promote the development of the sodium ion battery and promote the application of the sodium ion battery. The transition metal sulfide negative electrode material has high theoretical capacity, is simple to synthesize, and has huge application prospect in sodium ion batteries. In addition, with the development of flexible electronic books, flexible mobile phones and wearable electronic watches, and some portable medical electronic devices, the demand for flexible batteries is increasing. Therefore, the research and development of the high-capacity foldable flexible sodium-ion battery cathode material has important practical significance.
Disclosure of Invention
In order to solve the problems and the defects in the prior art, the invention aims to provide a preparation method of a flexible transition metal sulfide negative electrode material of a sodium ion battery, which is simple and easy to implement.
The purpose of the invention is realized by the following technical scheme.
The invention provides a preparation method of a flexible transition metal sulfide negative electrode material of a sodium ion battery, which comprises the following steps:
(1) weighing glucose, transition metal salt and thioacetamide according to the mass ratio of 1: 0.1-10: 0.01-10, sequentially adding the glucose, the transition metal salt and the thioacetamide into a mixed solvent consisting of a water-soluble organic solvent and deionized water, and uniformly dispersing to obtain a solution with the mass fraction of 3% -10%;
(2) soaking melamine sponge in the solution in the step (1), taking out, and drying in an oven at the temperature of 60-80 ℃ for 1-12 h to obtain a transition metal complex loaded by the melamine sponge;
(3) and (3) placing the prepared melamine sponge-loaded transition metal complex in a tubular furnace, and carrying out heat treatment for 1-4 h at the temperature of 300-800 ℃ in a flowing atmosphere to obtain the flexible transition metal sulfide negative electrode material.
Preferably, the anion of the transition metal salt in the step (1) comprises NO3 -、CO3 2-、CH3COO-、SO4 2-At least one of (1).
Preferably, the cation of the transition metal salt in the step (1) includes Mn2+、Fe3+、Co2+、Ni2+、Cu2+、Zn2+At least one of (1).
Preferably, the water-soluble organic solvent in step (1) includes one of alcohols with 1-6 carbon atoms.
Preferably, the volume ratio of the water-soluble organic solvent to the deionized water in the step (1) is 1: 0.1-10.
Preferably, the melamine sponge in the step (2) is soaked in the solution obtained in the step (1) for 0.01-1 h.
Preferably, the size of the melamine sponge in the step (2) is 300 × 300 cm.
Preferably, the gas introduced into the flowing atmosphere in the step (3) comprises at least one of hydrogen, argon and nitrogen.
Preferably, the temperature of the tube furnace in the step (3) is increased to 300-800 ℃ at a temperature increasing rate of 2-5 ℃/min.
Compared with the prior art, the invention has the following advantages and technical effects:
(1) the invention provides a simple and effective method, namely, the melamine sponge is used for absorbing solutions of different transition metal salts, and the flexible transition metal sulfide negative electrode material which is low in cost and easy for large-scale production is synthesized through calcination.
(2) The flexible transition metal sulfide negative electrode material is a self-supporting material, does not need a binder, a conductive agent and a coating process, can be directly used as a negative electrode material of a sodium ion battery, and is easy for industrial production.
(3) In the flexible transition metal sulfide negative electrode material, the carbonized melamine is used as a substrate, which is beneficial to keeping the flexibility of the battery during folding and bending; meanwhile, the transition metal sulfide grown on the substrate can increase the storage capacity of the flexible negative electrode, and the flexible transition metal sulfide negative electrode material shows excellent cycle performance and rate performance in the sodium ion battery.
Drawings
Fig. 1 is an SEM image of a flexible cobalt sulfide negative electrode material prepared in example 1;
FIG. 2 is a first charge-discharge curve of the flexible cobalt sulfide negative electrode material prepared in example 1 with a current density of 100 mA/g;
FIG. 3 is a graph of the cycle performance of the flexible cobalt sulfide negative electrode material prepared in example 1 at a current density of 1000 mA/g;
fig. 4 is a graph of rate performance of the flexible cobalt sulfide negative electrode material prepared in example 1;
fig. 5 is an SEM image of the flexible manganese sulfide negative electrode material prepared in example 2;
FIG. 6 is a graph of the cycle performance of the flexible manganese sulfide negative electrode material prepared in example 2 at a current density of 1000 mA/g;
fig. 7 is an SEM image of the flexible nickel sulfide negative electrode material prepared in example 3;
FIG. 8 is a graph of the cycle performance of the flexible nickel sulfide negative electrode material prepared in example 3 at a current density of 1000 mA/g.
Detailed Description
The present invention will be described in further detail with reference to examples, but the present invention is not limited to the examples.
The experimental procedures in the following examples are conventional unless otherwise specified.
Example 1
The embodiment provides a preparation method of a flexible transition metal sulfide negative electrode material of a sodium ion battery, which comprises the following steps:
1. weighing 1kg of glucose and 1kg of cobalt nitrate, and putting the glucose and the cobalt nitrate into a mixed solvent consisting of methanol and deionized water to be stirred and dissolved, wherein the volume ratio of the methanol to the deionized water is 1: 5.
2. Adding 1kg of thioacetamide, and continuing to magnetically stir for 1h to prepare a solution with the mass fraction of 3%.
3. 300 x 300cm melamine sponge was soaked in the above solution for 30 min.
4. And (3) taking out the melamine sponge, and drying in an oven at 60 ℃ for 1h to obtain the cobalt complex loaded by the melamine sponge.
5. And (3) heating the melamine sponge-loaded cobalt complex to 800 ℃ at a heating rate of 5 ℃/min in an argon atmosphere, and calcining for 4h to obtain the flexible cobalt sulfide negative electrode material.
The SEM image of the flexible cobalt sulfide negative electrode material obtained in this example is shown in fig. 1, and it can be seen from fig. 1 that cobalt sulfide particles are uniformly grown on the carbonized melamine sponge skeleton.
The flexible cobalt sulfide material is used as a negative electrode, the metal sodium is used as a positive electrode, the glass fiber is used as a diaphragm and NaClO4And (3) assembling the electrolyte into a sodium ion battery under an argon atmosphere. The battery is charged and discharged for the first time at a current density of 100mA/g between 0.01V and 3.0V, a charging and discharging curve is shown in figure 2, a charging and discharging platform of cobalt sulfide appears in the charging and discharging curve, and the cobalt sulfide participates in the desorption of sodium ions. The battery is subjected to a cycle performance test at a current density of 1000mA/g, a cycle curve is shown in figure 3, and as can be seen from the cycle curve, the flexible cobalt sulfide material has a reversible capacity of 415mAh/g after 100 cycles at the current density of 1000 mA/g. The battery was subjected to rate performance test, and the rate performance curve thereof is shown in fig. 4. As can be seen from the figure, the battery after loading cobalt sulfide has superior rate performance. The flexible cobalt sulfide material has a capacity of 295mAh/g at a current density of 3000 mA/g.
Example 2
The embodiment provides a preparation method of a flexible transition metal sulfide negative electrode material of a sodium ion battery, which comprises the following steps:
1. weighing 2kg of glucose and 8kg of manganese acetate, and putting the glucose and the manganese acetate into a mixed solvent consisting of ethanol and deionized water to be stirred and dissolved, wherein the volume ratio of the ethanol to the deionized water is 1: 2.
2. 18kg of thioacetamide is added to continue the magnetic stirring for 1 hour, and a solution with the mass fraction of 8% is prepared.
3. 300 x 300cm melamine sponge was soaked in the above solution for 10 min.
4. And (3) taking out the melamine sponge, and drying in an oven at 80 ℃ for 12h to obtain the manganese complex loaded by the melamine sponge.
5. And (3) heating the melamine sponge-loaded manganese complex to 600 ℃ at the heating rate of 2 ℃/min and calcining for 4h in the hydrogen atmosphere to obtain the flexible manganese sulfide negative electrode material.
The SEM image of the flexible manganese sulfide negative electrode material obtained in this example is shown in fig. 5, and it can be seen from fig. 5 that manganese sulfide particles uniformly grow on the carbonized melamine sponge skeleton.
The flexible manganese sulfide material is used as a negative electrode, the metal sodium is used as a positive electrode, the glass fiber is used as a diaphragm and NaClO4And (3) assembling the electrolyte into a sodium ion battery under an argon atmosphere. The battery is subjected to a cycle performance test at a current density of 1000mA/g, a cycle curve is shown in FIG. 6, and as can be seen from the cycle curve, the flexible manganese sulfide material has a reversible capacity of 460mAh/g after 100 cycles at the current density of 1000 mA/g.
Example 3
The embodiment provides a preparation method of a flexible transition metal sulfide negative electrode material of a sodium ion battery, which comprises the following steps:
1. 2kg of glucose and 10kg of nickel sulfate are weighed and put into a mixed solvent consisting of ethylene glycol and deionized water to be stirred and dissolved, wherein the volume ratio of the ethylene glycol to the deionized water is 1: 1.
2. 20kg of thioacetamide is added to continue magnetic stirring for 1 hour, and a solution with the mass fraction of 10% is prepared.
3. 300 x 300cm melamine sponge was soaked in the above solution for 5 min.
4. And taking out the melamine sponge, and drying in an oven at 60 ℃ for 12h to obtain the melamine sponge supported nickel complex.
5. And (3) heating the melamine sponge-loaded nickel complex to 500 ℃ at a heating rate of 3 ℃/min and calcining for 2h in a nitrogen atmosphere to obtain the flexible nickel sulfide negative electrode material.
The SEM image of the flexible nickel sulfide negative electrode material obtained in this example is shown in fig. 7, and it can be seen from fig. 7 that nickel sulfide particles uniformly grow on the carbonized melamine sponge skeleton. The flexible nickel sulfide material is used as a negative electrode, the metal sodium is used as a positive electrode, the glass fiber is used as a diaphragm and NaClO4And (3) assembling the electrolyte into a sodium ion battery under an argon atmosphere. The battery is subjected to a cycle performance test at a current density of 1000mA/g, a cycle curve is shown in FIG. 8, and as can be seen from the cycle curve, the flexible nickel sulfide material has a reversible capacity of 460mAh/g after 100 cycles at the current density of 1000 mA/g.
Comparative example 1
Heating the melamine sponge to 500 ℃ at the heating rate of 3 ℃/min and calcining for 2h under the nitrogen atmosphere to obtain the flexible negative electrode material. The flexible material is used as a negative electrode, the metal sodium is used as a positive electrode, the glass fiber is used as a diaphragm and NaClO4And (3) assembling the electrolyte into a sodium ion battery under an argon atmosphere. The battery is tested for cycle performance under the current density of 1000mA/g, and the cycle reversible capacity of the flexible negative electrode material is only 50mAh/g under the current density of 1000 mA/g. When the flexible negative electrode material is subjected to a rate performance test, the reversible capacity of the flexible material is only 3mAh/g under the current density of 3000mA/g of a battery. The invention provides a preparation method of a flexible transition metal sulfide negative electrode material of a sodium ion battery, the transition metal sulfide growing on a substrate can increase the storage capacity of the flexible negative electrode, and the flexible transition metal sulfide negative electrode material shows excellent cycle performance and rate capability in the sodium ion battery.
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 equivalent alterations, modifications or improvements made by those skilled in the art to the above-described embodiments using the technical solutions of the present invention are still within the scope of the technical solutions of the present invention.
Claims (7)
1. A preparation method of a flexible transition metal sulfide negative electrode material of a sodium ion battery is characterized by comprising the following steps:
(1) weighing glucose, transition metal salt and thioacetamide according to the mass ratio of 1 (0.1-10) to 0.01-10, sequentially adding the glucose, the transition metal salt and the thioacetamide into a mixed solvent consisting of a water-soluble organic solvent and deionized water, and uniformly dispersing to obtain a solution with the mass fraction of 3% -10%; the anion of the transition metal salt comprises NO3 -、CO3 2-、CH3COO-、SO4 2-At least one of; the cation of the transition metal salt includes Mn2+、Fe3+、Co2+、Ni2+、Cu2+、Zn2+At least one of;
(2) soaking melamine sponge in the solution in the step (1), taking out, and drying in an oven at the temperature of 60-80 ℃ for 1-12 h to obtain a transition metal complex loaded by the melamine sponge;
(3) and (3) placing the prepared melamine sponge-loaded transition metal complex in a tubular furnace, and calcining for 1-4 h at the temperature of 300-800 ℃ in a flowing atmosphere to obtain the flexible transition metal sulfide negative electrode material.
2. The preparation method of the flexible transition metal sulfide negative electrode material of the sodium-ion battery according to claim 1, wherein the water-soluble organic solvent in the step (1) comprises one of alcohols with 1-6 carbon atoms.
3. The preparation method of the flexible transition metal sulfide negative electrode material for the sodium-ion battery according to claim 1, wherein the volume ratio of the water-soluble organic solvent to the deionized water in the step (1) is 1 (0.1-10).
4. The preparation method of the flexible transition metal sulfide negative electrode material of the sodium-ion battery according to claim 1, wherein the melamine sponge in the step (2) is soaked in the solution obtained in the step (1) for 0.01-1 h.
5. The method for preparing the flexible transition metal sulfide anode material of the sodium-ion battery as claimed in claim 1, wherein the size of the melamine sponge in the step (2) is 300 x 300 cm.
6. The method for preparing the flexible transition metal sulfide anode material of the sodium-ion battery as claimed in claim 1, wherein the gas introduced into the flowing atmosphere in the step (3) comprises at least one of hydrogen, argon and nitrogen.
7. The preparation method of the flexible transition metal sulfide negative electrode material for the sodium-ion battery according to any one of claims 1 to 6, wherein the temperature of the tube furnace in the step (3) is raised to 300 to 800 ℃ at a temperature raising rate of 2 to 5 ℃/min.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH05314982A (en) * | 1992-05-07 | 1993-11-26 | Matsushita Electric Ind Co Ltd | Alkaline storage battery and manufacture thereof |
| CN101916854A (en) * | 2010-08-30 | 2010-12-15 | 上海交通大学 | Preparation method of zinc sulfide/carbon composite material for negative electrode of lithium ion battery |
| CN105140513A (en) * | 2015-07-23 | 2015-12-09 | 江苏新光环保工程有限公司 | MoS2/C lithium ion battery cathode composite material synthesized by taking carbohydrate as carbon source, and preparation method for MoS2/C lithium ion battery cathode composite material |
| CN107895786A (en) * | 2017-11-15 | 2018-04-10 | 晋中学院 | Flexible self-supporting SnS/ carbon foam composites and its preparation method and application |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH05314982A (en) * | 1992-05-07 | 1993-11-26 | Matsushita Electric Ind Co Ltd | Alkaline storage battery and manufacture thereof |
| CN101916854A (en) * | 2010-08-30 | 2010-12-15 | 上海交通大学 | Preparation method of zinc sulfide/carbon composite material for negative electrode of lithium ion battery |
| CN105140513A (en) * | 2015-07-23 | 2015-12-09 | 江苏新光环保工程有限公司 | MoS2/C lithium ion battery cathode composite material synthesized by taking carbohydrate as carbon source, and preparation method for MoS2/C lithium ion battery cathode composite material |
| CN107895786A (en) * | 2017-11-15 | 2018-04-10 | 晋中学院 | Flexible self-supporting SnS/ carbon foam composites and its preparation method and application |
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