CN114314664A - Vanadium oxide coated carbide composite material and preparation method and application thereof - Google Patents
Vanadium oxide coated carbide composite material and preparation method and application thereof Download PDFInfo
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- CN114314664A CN114314664A CN202111446322.5A CN202111446322A CN114314664A CN 114314664 A CN114314664 A CN 114314664A CN 202111446322 A CN202111446322 A CN 202111446322A CN 114314664 A CN114314664 A CN 114314664A
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Abstract
The invention discloses a vanadium oxide coated carbide composite material and a preparation method and application thereof. The invention reasonably utilizes the characteristic that vanadium carbide is easy to oxidize in air at a certain temperature, synthesizes the composite material of vanadium oxide coated carbide by adopting low-temperature annealing treatment, does not need to control oxygen partial pressure, namely the oxidation process is in an open air atmosphere, and the whole preparation method has the characteristics of easy operation, simple equipment, high efficiency, low cost and the like, and the prepared composite material powder has the characteristics of small particle size, high crystallinity and the like, and is suitable for being used as a cathode material of a lithium ion battery.
Description
Technical Field
The invention relates to the technical field of vanadium oxide coated carbide composite materials, in particular to a novel method for preparing composite material powder by low-temperature vanadium oxide carbide.
Background
The vanadium oxide has a unique crystal structure, high theoretical capacity, low cost and the like, and becomes a research hotspot of the lithium ion battery cathode material. However, the vanadium oxide exhibits poor rate performance and cycle stability in lithium ion batteries due to its low electronic conductivity and large volume deformation during cycling. At present, the electrochemical performance of vanadium oxide is improved by mainly utilizing a hydrothermal method and a template method to coat carbon on the surface of the vanadium oxide or constructing a compound of the vanadium oxide and the carbon material, but the methods have the defects of higher cost, more complex operation and the like, and the electrochemical performance of the obtained product is not ideal. Therefore, it is of no doubt important to explore new techniques for improving the electrochemical performance of vanadium oxides.
Disclosure of Invention
In view of the above-mentioned disadvantages, an object of the present invention is to provide a vanadium oxide-coated carbide composite material and a method for producing the same.
In order to achieve the purpose, the technical scheme provided by the invention is as follows:
a vanadium carbide is adopted as a raw material, the vanadium carbide is annealed at a low temperature in an air atmosphere to prepare the vanadium oxide coated carbide composite material, the temperature during the low-temperature annealing treatment is controlled to be 350-450 ℃, the time is less than or equal to 1 hour, the oxygen partial pressure is not required to be controlled, and the composite material is in an open air atmosphere. The vanadium carbide can be VC or V2C or mixtures of the two, e.g. using V2C (VC) is used as raw material. The vanadium oxide coating should not be too thick, which affects the conductivity, preferably not more than 1 μm.
The chemical formula of the composite material is VxOy@VaAnd C, wherein x is more than or equal to 1 and less than or equal to 6, y is more than or equal to 1 and less than or equal to 13, and a is 1 and 2. The composite material has the advantages of small particle size, high crystallinity and the like, and is suitable for being used as a negative electrode material of a lithium ion battery.
The vanadium oxide coated carbide composite material comprises an inner core part and an outer layer part coated on the inner core part, wherein the inner core part is vanadium carbide, and the outer layer part is vanadium oxide. The thickness of the outer layer portion is less than 1 micron.
The vanadium oxide coated carbide composite material is applied to a negative electrode material of a lithium ion battery.
The invention has the beneficial effects that: the invention reasonably utilizes the characteristic that vanadium carbide is easy to oxidize in air at a certain temperature, synthesizes the composite material of vanadium oxide coated carbide by adopting low-temperature annealing treatment, does not need to control oxygen partial pressure, namely the oxidation process is in an open air atmosphere, and the whole preparation method has the characteristics of easy operation, simple equipment, high efficiency, low cost and the like, and the prepared composite material powder has the characteristics of small particle size, high crystallinity and the like, and is suitable for being used as a cathode material of a lithium ion battery.
The invention is further illustrated below with reference to the figures and examples.
Drawings
FIG. 1 is a schematic flow chart of the present invention.
Fig. 2 is an XRD pattern of the vanadium oxide-coated carbide composite powder prepared in example 1.
FIG. 3 is an SEM topography of the vanadium oxide coated carbide composite powder prepared in example 1.
FIG. 4 is a SEM cross-sectional view of vanadium oxide coated carbide composite powder prepared in example 1.
Fig. 5 is a graph of rate performance of the vanadium oxide coated carbide composite material prepared in example 1 as a negative electrode material for a lithium ion battery.
Detailed Description
Example 1: this example provides a vanadium oxide coated carbide composite material and a method for preparing the same, wherein the vanadium oxide coated carbide composite material is prepared by mixing 80 wt.% V2Uniformly laying the mixture powder of C +20 wt.% VC in a corundum crucible, placing the corundum crucible in a stainless steel high-temperature tubular reaction furnace, heating to 400 ℃ at the speed of 5 ℃/min in the air atmosphere, and preserving heat for 1 h. And cooling the sample to room temperature along with the furnace, and taking out the sample to obtain the vanadium oxide coated carbide composite material. The XRD and surface SEM analysis results are shown in FIG. 2 and FIG. 3 respectivelyShown in the figure. The abscissa 2 θ in fig. 2 represents the diffraction angle (degree), and the ordinate Intensity represents the Intensity. The results of the SEM cross-sectional analysis of fig. 4 show that the vanadium oxide is wrapped in the outer layer of vanadium carbide in the resulting product. Taking the prepared composite material as an active substance, and mixing the active substance with carbon black and PVDF in a mass ratio of 7: 2: 1 as electrode plate, using lithium plate as counter electrode, using porous polypropylene as diaphragm, 1mol/L LiPF6The electrolyte is assembled into a button cell in a glove box with the partial pressure of water and oxygen lower than 0.01ppm, and the figure 5 shows the result of the rate performance test.
Example 2: this example provides a vanadium oxide coated carbide composite material and a method for preparing the same, wherein the vanadium oxide coated carbide composite material is prepared by mixing 90 wt.% V2C. Uniformly laying 10 wt.% VC mixture powder in a corundum crucible, placing the corundum crucible in a stainless steel high-temperature tubular reaction furnace, heating to 350 ℃ at the speed of 5 ℃/min in the air atmosphere, and preserving heat for 1 h. And cooling the sample to room temperature along with the furnace, and taking out the sample to obtain the vanadium oxide coated carbide composite material.
Example 3: this example provides a vanadium oxide coated carbide composite material and a method for preparing the same, which comprises mixing V2And C powder is uniformly laid in a corundum crucible, is placed in a stainless steel high-temperature tubular reaction furnace, is heated to 350 ℃ at the speed of 5 ℃/min in the air atmosphere, and is kept for 0.5 h. And cooling the sample to room temperature along with the furnace, and taking out the sample to obtain the vanadium oxide coated carbide composite material.
Example 4: the embodiment provides a vanadium oxide coated carbide composite material and a preparation method thereof, wherein VC powder is uniformly laid in a corundum crucible, is placed in a stainless steel high-temperature tubular reaction furnace, and is heated to 400 ℃ at the speed of 5 ℃/min in the air atmosphere and is kept warm for 40 min. And cooling the sample to room temperature along with the furnace, and taking out the sample to obtain the vanadium oxide coated carbide composite material.
Example 5: this example provides a vanadium oxide coated carbide composite material and a method for preparing the same, which comprises mixing V2Uniformly spreading the C powder in a corundum crucible, placing the corundum crucible in a stainless steel high-temperature tubular reaction furnace, and heating to 4 ℃ at the speed of 5 ℃/min in the air atmosphereKeeping the temperature at 50 ℃ for 20 min. And cooling the sample to room temperature along with the furnace, and taking out the sample to obtain the vanadium oxide coated carbide composite material.
Example 6: this example provides a vanadium oxide coated carbide composite material and a method for preparing the same, wherein the vanadium oxide coated carbide composite material is prepared by mixing 70 wt.% V2C. Uniformly laying the mixture powder of 30 wt.% VC in a corundum crucible, placing the corundum crucible in a stainless steel high-temperature tubular reaction furnace, heating to 400 ℃ at the speed of 5 ℃/min in the air atmosphere, and preserving heat for 45 min. And cooling the sample to room temperature along with the furnace, and taking out the sample to obtain the vanadium oxide coated carbide composite material.
Example 7: the embodiment provides a vanadium oxide coated carbide composite material and a preparation method thereof, wherein VC powder is uniformly laid in a corundum crucible, is placed in a stainless steel high-temperature tubular reaction furnace, is heated to 350 ℃ at the speed of 5 ℃/min in the air atmosphere, and is kept warm for 0.5 h. And cooling the sample to room temperature along with the furnace, and taking out the sample to obtain the vanadium oxide coated carbide composite material.
Example 8: this example provides a vanadium oxide coated carbide composite material and a method for preparing the same, which comprises mixing V2And C powder is uniformly laid in a corundum crucible, is placed in a stainless steel high-temperature tubular reaction furnace, is heated to 420 ℃ at the speed of 5 ℃/min in the air atmosphere, and is kept for 0.5 h. And cooling the sample to room temperature along with the furnace, and taking out the sample to obtain the vanadium oxide coated carbide composite material.
The above examples are only preferred embodiments of the present invention, and the present invention is not limited to all embodiments, and any technical solution using one of the above examples or equivalent changes made according to the above examples is within the scope of the present invention. The method reasonably utilizes the characteristic that vanadium carbide is easily oxidized in air at a certain temperature, synthesizes the vanadium oxide carbide-coated composite material by adopting low-temperature annealing treatment, does not need to control oxygen partial pressure, has the characteristics of easiness in operation, simple equipment, high efficiency, low cost and the like, and the prepared composite material powder has the characteristics of small particle size, high crystallinity and the like.
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. Other composite materials and methods of making the same, using the same or similar procedures as described in the above examples of the invention, are within the scope of the invention.
Claims (8)
1. A preparation method of a vanadium oxide coated carbide composite material is characterized in that vanadium carbide is adopted as a raw material, and the vanadium oxide coated carbide composite material is prepared after low-temperature annealing treatment in an air atmosphere.
2. The method for preparing the vanadium oxide-coated carbide composite material according to claim 1, wherein the temperature of the low-temperature annealing treatment is 350 to 450 ℃.
3. The method for preparing a vanadium oxide-coated carbide composite material according to claim 1 or 2, wherein the time of the low-temperature annealing treatment is 1 hour or less.
4. The method of preparing a vanadium oxide-coated carbide composite material according to claim 1, wherein the vanadium carbide is VC or V2C or a mixture of the two.
5. The method of preparing a vanadium oxide-coated carbide composite material according to claim 2, wherein the composite material has a chemical formula of VxOy@VaAnd C, wherein x is more than or equal to 1 and less than or equal to 6, y is more than or equal to 1 and less than or equal to 13, and a is 1 and 2.
6. The method of making a vanadium oxide-coated carbide composite material according to claim 1, wherein the vanadium oxide coating has a thickness of less than 1 micron.
7. A vanadium oxide-coated carbide composite material, characterized in that it is produced by the method for producing a vanadium oxide-coated carbide composite material according to any one of claims 1 to 6, comprising an inner core portion and an outer layer portion coated on the inner core portion, wherein the inner core portion is vanadium carbide and the outer layer portion is vanadium oxide.
8. The vanadium oxide-coated carbide composite material according to any one of claims 1 to 6 or claim 7, which is applied to a negative electrode material of a lithium ion battery.
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| CN115010502A (en) * | 2022-05-25 | 2022-09-06 | 松山湖材料实验室 | Method for rapidly preparing nano vanadium nitride coated carbon fiber composite ceramic powder, product and application thereof |
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