CN111924873A - Novel sodium-ion battery negative electrode material and preparation method thereof - Google Patents
Novel sodium-ion battery negative electrode material and preparation method thereof Download PDFInfo
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G19/00—Compounds of tin
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/05—Preparation or purification of carbon not covered by groups C01B32/15, C01B32/20, C01B32/25, C01B32/30
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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
- 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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- 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
- H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
- H01M4/628—Inhibitors, e.g. gassing inhibitors, corrosion inhibitors
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/80—Particles consisting of a mixture of two or more inorganic phases
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/40—Electric properties
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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
- H01M2004/021—Physical characteristics, e.g. porosity, surface area
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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
- H01M2004/026—Electrodes composed of, or comprising, active material characterised by the polarity
- H01M2004/027—Negative electrodes
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
Abstract
The invention discloses a novel sodium ion battery cathode material and a preparation method thereof, which comprises the steps of firstly dissolving a sulfur source, a tin source and a carbon source in water to obtain a mixed solution; adsorbing the mixed solution by using a foam material, and then freezing and drying to obtain a precursor; then transferring the precursor into a microwave reactor, and performing microwave irradiation under an inert condition to obtain an intermediate product; and finally, uniformly mixing the intermediate product with selenium powder, and performing high-temperature treatment under the protection of inert gas to obtain the novel sodium-ion battery cathode material. According to the invention, the activity of the battery cathode material is enhanced through selenium doping and desulfurization, a certain reserved space is provided for the deintercalation of sodium ions in the battery cathode, the volume expansion and pulverization of the electrode cathode material caused by the deintercalation of the sodium ions are avoided, and the electrochemical performance and the cycle performance of the sodium ion battery cathode material are improved.
Description
Technical Field
The invention belongs to the technical field of nano materials, and particularly relates to a novel sodium-ion battery cathode material and a preparation method thereof.
Background
The sodium ion battery is a very cost-effective substitute of the lithium ion battery due to the easily available raw materials and low price, the working principle of the sodium ion battery is similar to that of the lithium ion battery, when in charging, Na + is extracted from the positive electrode and is inserted into the negative electrode through the electrolyte,the reverse is true when discharging, by storing and releasing electrical energy by transfer via sodium ions. The prior sodium ion negative electrode material is mainly concentrated in the fields of carbon materials, transition metals and alloy compounds thereof, such as carbon materials of hard carbon, hollow carbon spheres, carbon fibers and the like, Sn and SnO2，Bi0.94Sb1.06S3And metal/metal chalcogenides such as Sb. However, these negative electrode materials have large volume change in the electrochemical reaction process, and the structure is easily damaged after many times of charging and discharging, and the cycle performance is poor.
Disclosure of Invention
Based on the defects of the prior art, the invention aims to provide a novel sodium-ion battery cathode material and a preparation method thereof, which are used for solving the problem of low electrochemical performance caused by the structural expansion of the cathode material in the prior art.
In order to achieve the purpose, the invention adopts the following technical scheme.
A preparation method of a novel sodium-ion battery negative electrode material comprises the following steps:
the method comprises the following steps: dissolving a sulfur source, a tin source and a carbon source in water to obtain a mixed solution; adsorbing the mixed solution by using a foam material, and then freezing and drying to obtain a precursor; transferring the precursor into a microwave reactor, and performing microwave irradiation under an inert condition to obtain an intermediate product; and step four, uniformly mixing the intermediate product with selenium powder, and performing high-temperature treatment under the protection of inert gas to obtain the novel sodium-ion battery cathode material.
As an improved technical scheme of the invention, in the first step, the sulfur source is one of water-soluble sulfate and sodium thiosulfate. The sulfate mainly comprises one or more of sodium sulfate, potassium sulfate, lithium sulfate, magnesium sulfate, nickel sulfate, ferrous sulfate, zinc sulfate, aluminum sulfate and copper sulfate. The tin source is mainly a water-soluble tin salt, such as one of tin tetrachloride and tin methane sulfonate. The carbon source is mainly a water-soluble organic carbon source, such as one or more of sucrose, glucose, phenolic resin, epoxy resin, agar, polyaniline and polypyrrole.
As an improved technical scheme of the invention, the molar ratio of the sulfur source to the tin source to the carbon source is 2-3: 1: 0.5 to 1.5, and the concentration of the tin source in the mixed solution is 0.1 to 1 mol/L.
As an improved technical scheme of the invention, the foam material is melamine foam material.
As an improved technical scheme of the invention, in the second step, the freeze drying temperature is-50 to-30 ℃.
As an improved technical scheme of the invention, in the third step, after introducing inert gas into the microwave reactor for at least 30min, the precursor is added, the microwave irradiation power is 800-1200W, and the duration is 1-30 min.
As an improved technical scheme of the invention, in the fourth step, the mass ratio of the intermediate product to the selenium powder is 10: 0.1 to 1.
According to the improved technical scheme, in the fourth step, the intermediate product and selenium powder are subjected to heat preservation for 4-6 hours at 500-700 ℃ under the protection of nitrogen, so that the novel sodium-ion battery cathode material is obtained.
The invention also provides a novel sodium-ion battery cathode material prepared by the method.
Advantageous effects
The invention provides a novel sodium-ion battery cathode material and a preparation method thereof. The sulfur source, the tin source and the carbon source are fully dispersed and adsorbed in the holes of the foam material, and the foam material avoids the aggregation of reaction products, thereby being beneficial to S simple substance and SnS2The nano-scale in-situ reaction grows and disperses in the carbon material. The microwave reactor provides ultra-fast temperature rise speed, greatly shortens the reaction time, avoids the migration and agglomeration of metal atoms, and is favorable for forming nano-scale S simple substance and SnS with smaller particle size2A compound is provided. In a tube furnace, the intermediate product is reacted with selenium powder in SnS2Se is doped on the surface, S simple substance is sublimated and removed, a porous structure is formed in the sodium ion battery cathode material, an ion containing space is provided for the sodium ion battery cathode material in the charging and discharging process, the volume expansion and pulverization caused by the desorption of sodium ions of the electrode material are avoided, and the sodium ion battery cathode material is improvedThe cycle performance of the material.
Detailed Description
The present invention will now be described in detail with reference to specific embodiments thereof for the purpose of clearly understanding the present invention by those skilled in the art.
Example 1
A sulfur source, a tin source and a carbon source are mixed according to a molar ratio of 2.5: 1: 1 in water to obtain a mixed solution in which the concentration of the tin source is 0.5 mol/L. The sulfur source is sodium sulfate, the tin source is tin tetrachloride, and the carbon source is glucose. And (3) immersing the melamine foam material into the mixed solution, repeatedly pressing and absorbing until the melamine foam material is saturated, and then putting the melamine foam material into a freeze dryer at the temperature of minus 40 ℃ for freeze drying for 48 hours to obtain a precursor. And introducing inert gas into the microwave reactor for at least 30min, then adding the precursor, and performing microwave irradiation with the microwave irradiation power of 1000W and the time of 5min to obtain an intermediate product. And fully and uniformly mixing the intermediate product with selenium powder. The mixing mode preferably adopts a ball mill, the parameters of the ball mill are adjusted, and the ball-powder ratio is 15: 1, the rotating speed is 200r/min, and the ball milling time is 4 h. And transferring the mixed intermediate product and selenium powder to a tubular furnace, and preserving heat for 5 hours at 600 ℃ by taking nitrogen as protective gas to obtain the novel sodium-ion battery cathode material.
Example 2
The present embodiment is different from embodiment 1 in that: the molar ratio of the sulfur source to the tin source to the carbon source is 1: 1: 1, the rest is the same as embodiment 1, and the description is omitted here.
Example 3
The present embodiment is different from embodiment 1 in that: the molar ratio of the sulfur source to the tin source to the carbon source is 2: 1: 0.5, as in example 1, and will not be described herein.
Example 4
The present embodiment is different from embodiment 1 in that: the molar ratio of the sulfur source to the tin source to the carbon source is 3: 1: 1.5, the rest is the same as example 1, and the description is omitted here.
Example 5
The present embodiment is different from embodiment 1 in that: the concentration of the tin source was 0.1mol/L, and the rest of the process was the same as example 1, and will not be described herein.
Example 6
The present embodiment is different from embodiment 1 in that: the concentration of the tin source was 1mol/L, and the rest of the process was the same as example 1, and will not be described again here.
Example 7
The present embodiment is different from embodiment 1 in that: the sulfur source is sodium thiosulfate, the tin source is tin methanesulfonate, and the carbon source is polypyrrole, which is the same as in example 1 and is not described herein again.
Example 8
This example is different from example 1 in that the freeze-drying temperature is-50 deg.C, and the rest is the same as example 1, and will not be described herein.
Example 9
This example is different from example 1 in that the freeze-drying temperature is-30 deg.C, and the rest is the same as example 1, and will not be described herein.
Example 10
The difference between this embodiment and embodiment 1 is that the microwave irradiation power is 800W, and the duration is 30min, which is the same as embodiment 1 and will not be described herein again.
Example 11
The difference between this embodiment and embodiment 1 is that the microwave irradiation power is 1200W, and the duration is 1min, which is the same as embodiment 1 and will not be described herein again.
Example 12
The difference between the embodiment and the embodiment 1 is that the mass ratio of the intermediate product to the selenium powder is 10: 0.1, as in example 1, and will not be described herein.
Example 13
The difference between the embodiment and the embodiment 1 is that the mass ratio of the intermediate product to the selenium powder is 10: 0.3, as in example 1, and will not be described herein.
Example 14
The difference between the embodiment and the embodiment 1 is that the mass ratio of the intermediate product to the selenium powder is 10: 0.7, as in example 1, and will not be described herein.
Example 15
The difference between the embodiment and the embodiment 1 is that the mass ratio of the intermediate product to the selenium powder is 10: 1, the rest is the same as embodiment 1, and the description is omitted here.
Example 16
The difference between this example and example 1 is that the intermediate product and selenium powder are kept at 500 ℃ for 6h under the protection of nitrogen, and the rest is the same as example 1, and will not be described herein again.
Example 17
The difference between this example and example 1 is that the intermediate product and selenium powder are kept at 700 ℃ for 4h under the protection of nitrogen, and the rest is the same as example 1, and will not be described herein again.
Example 18
The difference between this example and example 1 is that the mixed solution is directly freeze-dried to obtain a precursor, and the rest is the same as example 1, and will not be described herein again.
Example 19
The difference between this example and example 1 is that the intermediate product was directly transferred to a tube furnace, and the intermediate product was kept at 600 ℃ for 5 hours under nitrogen as a protective gas, and the rest of this example is the same as example 1 and will not be described herein again.
Preparing a negative pole piece: the novel lithium ion battery negative electrode material, acetylene black and PVDF are mixed according to the mass ratio of 8: 1: 1 grinding in a mortar for more than 20min to fully mix the three. Adding a proper amount of N-methyl pyrrolidone (NMP) dropwise and stirring for 8h at room temperature under the action of a magnetic stirrer to obtain a paste material. The paste was poured onto a current collector (copper foil) uniformly and the pole piece was coated with a thickness of about 150 μm using a hand coater. Drying at 80 deg.C for 12h, and drying at 120 deg.C for 12 h. The circular pole pieces, with a diameter of about 1.2cm, were cut by a microtome and left to be assembled into button cells.
Assembling the sodium-ion button cell: the button cell is of a CR2016 type and is assembled in a glove box. The protective gas in the glove box is argon, and the partial pressure of water and oxygen is lower than 1 ppm. Sequentially assembling the positive shell, the gasket, the sodium sheet, the diaphragm, the negative pole piece and the gasket which are matched with the CR2016, and dropwise adding a proper amount of electrolyte among the sodium sheet, the diaphragm and the negative pole piece to enable the electrolyte to fully infiltrate the diaphragm and the negative pole piece. And finally, sealing and compacting the assembled analog button cell under the pressure of about 4 Mpa. The assembled cell was left to stand at room temperature for 8-12 hours for testing. The specific capacity of each example measured at a current density of 100mA/g is shown in the following table.
Variations and modifications to the above-described embodiments may occur to those skilled in the art, which fall within the scope and spirit of the above description. Therefore, the present invention is not limited to the specific embodiments disclosed and described above, and some modifications and variations of the present invention should fall within the scope of the claims of the present invention. Furthermore, although specific terms are employed herein, they are used in a generic and descriptive sense only and not for purposes of limitation.
Claims (9)
1. A preparation method of a novel sodium-ion battery negative electrode material comprises the following steps:
the method comprises the following steps: dissolving a sulfur source, a tin source and a carbon source in water to obtain a mixed solution;
adsorbing the mixed solution by using a foam material, and then freezing and drying to obtain a precursor;
transferring the precursor into a microwave reactor, and performing microwave irradiation under an inert condition to obtain an intermediate product;
and step four, uniformly mixing the intermediate product with selenium powder, and performing high-temperature treatment under the protection of inert gas to obtain the novel sodium-ion battery cathode material.
2. The preparation method of the novel sodium-ion battery anode material according to claim 1, characterized by comprising the following steps: in the first step, the sulfur source is one of water-soluble sulfate and sodium thiosulfate; the tin source is mainly water-soluble tin salt; the carbon source is mainly a water-soluble organic carbon source.
3. The preparation method of the novel sodium-ion battery anode material according to claim 1, characterized by comprising the following steps: the molar ratio of the sulfur source to the tin source to the carbon source is 2-3: 1: 0.5 to 1.5, and the concentration of the tin source in the mixed solution is 0.1 to 1 mol/L.
4. The preparation method of the novel sodium-ion battery anode material according to claim 1, characterized by comprising the following steps: the foam material is melamine foam material.
5. The preparation method of the novel sodium-ion battery anode material according to claim 1, characterized by comprising the following steps: in the second step, the freeze drying temperature is-50 to-30 ℃.
6. The preparation method of the novel sodium-ion battery anode material according to claim 1, characterized by comprising the following steps: and in the third step, after introducing inert gas into the microwave reactor for at least 30min, adding the precursor, wherein the microwave irradiation power is 800-1200W, and the duration is 1-30 min.
7. The preparation method of the novel sodium-ion battery anode material according to claim 1, characterized by comprising the following steps: in the fourth step, the mass ratio of the intermediate product to the selenium powder is 10: 0.1 to 1.
8. The preparation method of the novel sodium-ion battery anode material according to claim 1, characterized by comprising the following steps: and in the fourth step, the intermediate product and selenium powder are subjected to heat preservation for 4-6 hours at 500-700 ℃ under the protection of nitrogen, so as to obtain the novel sodium-ion battery cathode material.
9. A novel sodium-ion battery negative electrode material prepared by the preparation method of the novel sodium-ion battery negative electrode material as claimed in any one of claims 1 to 8.
Priority Applications (2)
| Application Number | Priority Date | Filing Date | Title |
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| CN202010764800.6A CN111924873A (en) | 2020-07-31 | 2020-07-31 | Novel sodium-ion battery negative electrode material and preparation method thereof |
| PCT/CN2020/124576 WO2022021642A1 (en) | 2020-07-31 | 2020-10-29 | Sodium ion battery negative electrode material and preparation method therefor |
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| CN202010764800.6A CN111924873A (en) | 2020-07-31 | 2020-07-31 | Novel sodium-ion battery negative electrode material and preparation method thereof |
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| WO2022021642A1 (en) * | 2020-07-31 | 2022-02-03 | 广东凯金新能源科技股份有限公司 | Sodium ion battery negative electrode material and preparation method therefor |
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| CN115692612A (en) * | 2022-11-03 | 2023-02-03 | 福州大学 | Tin-carbon negative electrode material and preparation method thereof |
| CN115594156B (en) * | 2022-11-10 | 2023-11-28 | 安徽工业大学 | Bamboo-like antimony-antimony sulfide selenide@hollow carbon tube material and preparation method and application thereof |
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- 2020-10-29 WO PCT/CN2020/124576 patent/WO2022021642A1/en active Application Filing
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