CN114314664B - 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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- CN114314664B CN114314664B CN202111446322.5A CN202111446322A CN114314664B CN 114314664 B CN114314664 B CN 114314664B CN 202111446322 A CN202111446322 A CN 202111446322A CN 114314664 B CN114314664 B CN 114314664B
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Abstract
The invention discloses a vanadium oxide coated carbide composite material, a preparation method and application thereof. The invention reasonably utilizes the characteristic that vanadium carbide is easy to oxidize in air with 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, thereby being suitable for serving 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
Vanadium oxide has become a research hot spot of lithium ion battery anode materials with unique crystal structure, high theoretical capacity, low cost and the like. However, in view of its low electron conductivity and large volume deformation in the cycle, vanadium oxide exhibits poor rate performance and cycle stability in lithium ion batteries. At present, the electrochemical performance of the vanadium oxide is improved by mainly coating the surface of the vanadium oxide with carbon or constructing a compound of the vanadium oxide and a carbon material by using a hydrothermal method and a template method, 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 significant to explore new technologies for improving the electrochemical performance of vanadium oxides.
Disclosure of Invention
In view of the above-mentioned shortcomings, the present invention aims to provide a vanadium oxide coated carbide composite material and a preparation method thereof.
In order to achieve the above purpose, the technical scheme provided by the invention is as follows:
the preparation method of the vanadium oxide coated carbide composite material adopts vanadium carbide as a raw material, and the vanadium oxide coated vanadium carbide composite material is prepared after low-temperature annealing treatment in an air atmosphere, wherein the temperature is controlled to be 350-450 ℃ during the low-temperature annealing treatment, the time is less than or equal to 1 hour, the oxygen partial pressure is not required to be controlled, and the vanadium oxide coated carbide composite material is in an open air atmosphere. The vanadium carbide can be VC, V 2 C or mixtures of both, e.g. using V 2 C (VC) is used as a raw material. The coating of the vanadium oxide is not too thick, but too thick affects the conductivity, preferably not more than 1 μm.
The chemical formula of the composite material is V x O y @V a 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 more than or equal to 1 and 2. The composite material has the advantages of small particle size, higher crystallinity and the like, and is suitable for serving as a negative electrode material of a lithium ion battery.
The vanadium oxide coated carbide composite material comprises a core part and an outer layer part coated on the core part, wherein the 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 beneficial effects of the invention are as follows: the invention reasonably utilizes the characteristic that vanadium carbide is easy to oxidize in air with 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, thereby being suitable for serving as a cathode material of a lithium ion battery.
The invention will be further described with reference to the drawings 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 morphology of the vanadium oxide coated carbide composite powder prepared in example 1.
Fig. 4 is an SEM cross-sectional view of the vanadium oxide coated carbide composite powder prepared in example 1.
Fig. 5 is a graph showing the 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: the embodiment provides a vanadium oxide coated carbide composite material and a preparation method thereof, wherein the mass ratio is 80wt.% V 2 The mixture powder of C+20wt.% VC is uniformly laid in a corundum crucible, and is placed in a stainless steel high-temperature tubular reaction furnace, and is heated to 400 ℃ at a rate of 5 ℃/min in an air atmosphere and is kept for 1h. 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 3, respectively. The abscissa 2θ in fig. 2 represents the diffraction angle (degree), and the ordinate Intensity represents the Intensity. The result of SEM cross-section analysis of fig. 4 shows that the vanadium oxide in the obtained product is coated on the outer layer of vanadium carbide. The prepared composite material is used as an active substance, and is mixed with carbon black and PVDF according to the mass ratio of 7:2:1, a lithium sheet is used as a counter electrode, porous polypropylene is used as a diaphragm, and 1mol/L LiPF is used as a cathode 6 As an electrolyte, a button cell was assembled in a glove box with water and oxygen partial pressures of less than 0.01ppm, and fig. 5 shows the results of the rate performance test.
Example 2: the present embodiment provides a vanadium oxide coated carbonCompound composite material and its preparation method, the mass ratio is 90wt.% V 2 C. 10wt.% of VC mixture powder is uniformly laid in a corundum crucible, placed in a stainless steel high-temperature tubular reaction furnace, heated to 350 ℃ at a rate of 5 ℃/min in an air atmosphere and kept for 1h. 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: the embodiment provides a vanadium oxide coated carbide composite material and a preparation method thereof, wherein V is as follows 2 The powder C is evenly spread in a corundum crucible and is placed in a stainless steel high-temperature tubular reaction furnace, and the temperature is raised to 350 ℃ at a speed of 5 ℃/min and is kept for 0.5h in an air atmosphere. 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, VC powder is uniformly laid in a corundum crucible and is placed in a stainless steel high-temperature tubular reaction furnace, and the temperature is raised to 400 ℃ at a speed of 5 ℃/min in an air atmosphere and is kept for 40min. 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: the embodiment provides a vanadium oxide coated carbide composite material and a preparation method thereof, wherein V is as follows 2 The powder C is evenly spread in a corundum crucible, and is placed in a stainless steel high-temperature tubular reaction furnace, and is heated to 450 ℃ at a speed of 5 ℃/min in an air atmosphere, and is kept for 20min. 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: the embodiment provides a vanadium oxide coated carbide composite material and a preparation method thereof, wherein the mass ratio is 70wt.% V 2 C. The 30wt.% of VC mixture powder is uniformly laid in a corundum crucible and placed in a stainless steel high-temperature tubular reaction furnace, and the temperature is raised to 400 ℃ at a rate of 5 ℃/min in an air atmosphere and kept for 45min. 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, VC powder is uniformly laid in a corundum crucible and is placed in a stainless steel high-temperature tubular reaction furnace, and the temperature is raised to 350 ℃ at a speed of 5 ℃/min in an air atmosphere and is kept for 0.5h. 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: the embodiment provides a vanadium oxide coated carbide composite material and a preparation method thereof, wherein V is as follows 2 The powder C is evenly spread in a corundum crucible and is placed in a stainless steel high-temperature tubular reaction furnace, and the temperature is raised to 420 ℃ at a speed of 5 ℃/min in an air atmosphere and is kept for 0.5h. 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 the embodiments, but the technical solution of one of the above examples or the equivalent changes according to the above examples are all within the scope of the present invention. The invention reasonably utilizes the characteristic that vanadium carbide is easy to oxidize in air with 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, 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.
Variations and modifications to the above would be obvious to persons skilled in the art to which the invention pertains from the foregoing description and teachings. Therefore, the invention is not limited to the specific embodiments disclosed and described above, but some modifications and changes of the invention should be also included in the scope of the claims of the invention. In addition, although specific terms are used in the present specification, these terms are for convenience of description only and do not limit the present invention in any way. As described in the above embodiments of the present invention, other composite materials obtained by the same or similar steps and the preparation method thereof are all within the scope of the present invention.
Claims (3)
1. The preparation method of the 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 without controlling oxygen partial pressure and is in an open air atmosphere;
the temperature of the low-temperature annealing treatment is 350-450 ℃;
the time of the low-temperature annealing treatment is less than or equal to 1 hour;
the vanadium carbide is VC, V 2 C a mixture of both;
the chemical formula of the composite material is V x O y @V a 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=1 and 2;
the vanadium oxide coating has a thickness of less than 1 micron.
2. The vanadium oxide coated carbide composite material is characterized by being prepared by the preparation method of the vanadium oxide coated carbide composite material according to claim 1, and comprising a core part and an outer layer part coated on the core part, wherein the core part is vanadium carbide, and the outer layer part is vanadium oxide.
3. A vanadium oxide coated carbide composite material prepared by the preparation method of claim 1 or a vanadium oxide coated carbide composite material of claim 2 is applied to a negative electrode material of a lithium ion battery.
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