CN114864916A - Niobium pentoxide coated graphite composite negative electrode material and preparation method thereof - Google Patents
Niobium pentoxide coated graphite composite negative electrode material and preparation method thereof Download PDFInfo
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Abstract
The invention relates to the technical field of electrochemical devices and discloses a niobium pentoxide coated graphite composite negative electrode material, wherein the mass ratio of niobium pentoxide is 1-15 wt%, the niobium pentoxide forms uniformly distributed coating layers on the graphite negative electrode material, and the graphite negative electrode material is spherical particles of 5-15 mu m. The invention also discloses a preparation method of the niobium pentoxide coated graphite composite negative electrode material. The niobium pentoxide coated graphite composite negative electrode material and the preparation method thereof can obviously reduce the interface resistance and improve the cycle stability and the quick charging capability of the graphite negative electrode material, and the method is simple, low in cost and capable of realizing large-scale production.
Description
Technical Field
The invention relates to the technical field of electrochemical devices, in particular to a niobium pentoxide coated graphite composite negative electrode material and a preparation method thereof.
Background
With the over-development of fossil energy, the increasing shortage of non-renewable resources and the gradual deterioration of ecological environment, the energy crisis and environmental pollution problems have become the problems that people pay attention to and need to solve. Therefore, the development of clean and renewable green new energy sources and high-performance energy storage devices has become a research hotspot in all countries of the world. As a new generation of green energy storage and conversion devices, lithium ion batteries have the advantages of high energy density, long cycle life, high discharge voltage, no memory effect, low self-discharge rate, small environmental pollution and the like, and have been widely applied to the fields of portable electronic equipment, large-scale energy storage systems, power automobiles and the like. However, the endurance mileage of a lithium ion battery of a pure electric vehicle has a certain gap compared with that of a conventional fuel vehicle. At present, the problem of endurance is solved mainly from two major aspects of improving the battery capacity and improving the charging speed of the battery. Therefore, the development of lithium ion batteries having both high power density and high energy density is urgent.
In order to solve these problems, researchers have made great efforts in recent years to develop graphite anode materials of high power density and high energy density. The graphite material has the advantages of excellent conductivity, stable charge and discharge platform, good lithium ion intercalation-deintercalation capability, abundant resources, low cost and the like, and is the most successful cathode material in commercial application at present. However, as people demand high-power and high-energy-density lithium ion batteries more and more urgently, the traditional graphite cathode material faces huge challenges, such as fast charging, high safety performance, high energy density, high power density and the like.
In order to solve the above problems, researchers have proposed a variety of coping strategies, mainly including four strategies of pore structure change, surface modification, element doping, and surface coating.Among them, surface coating is widely used to improve the cycle stability, and among them, the surface coating modification using oxide material is the most common, and most typical is Al 2 O 3 、SnO 2 、TiO 2 And the like. However, these metal oxides have low electron conductivity and cannot improve the rapid charging ability of graphite.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provides a niobium pentoxide coated graphite composite negative electrode material and a preparation method thereof, which can obviously reduce the interface resistance and improve the cycle stability and the quick charging capability of the graphite negative electrode material, and the method is simple, has lower cost and can be used for large-scale production.
In order to achieve the purpose, the niobium pentoxide-coated graphite composite negative electrode material is designed, the mass ratio of the niobium pentoxide is 1-15 wt%, the niobium pentoxide forms a uniformly distributed coating layer on the graphite negative electrode material, and the graphite negative electrode material is spherical particles with the particle size of 5-15 microns.
The preparation method of the niobium pentoxide coated graphite composite negative electrode material comprises the following steps:
A) dissolving niobium pentachloride in absolute ethyl alcohol to form a niobium alcohol solution;
B) dropwise adding deionized water into the niobium alcohol solution prepared in the step A), and uniformly stirring to form a mixed solvent;
C) adding graphite into the mixed solvent prepared in the step B) according to the molar ratio of niobium to graphite in the claim 1, uniformly stirring, evaporating the solvent to dryness in a water bath, putting the solvent into an oven for drying, and grinding the solvent into powder;
D) sintering the powder prepared in the step C) in a tubular furnace to obtain the niobium pentoxide coated graphite composite negative electrode material.
Preferably, in the step A), the solid-liquid mass ratio of the niobium alcohol solution is 1-15: 155.
preferably, in the step B), in the mixed solvent, the ratio of the sum of the masses of the deionized water and the absolute ethyl alcohol to the mass of the niobium pentachloride is 205: (1-15).
Preferably, in the step C), the graphite is spherical particles of 5-15 μm, the temperature of the water bath is 70-80 ℃, the stirring speed in the water bath is 300-600 r/min until the solvent is evaporated, and the temperature of the oven is 50-80 ℃.
Preferably, in the step D), the sintering is performed for 2-3 hours in an argon atmosphere at a heating rate of 2-10 ℃ per min to 700-900 ℃.
The principle of the invention is as follows: nb 2 O 5 The graphite cathode material has excellent rate capability and good safety performance, and is coated on the surface of a graphite cathode material to form a core-shell structure, so that the interface impedance can be reduced, the cycle stability and the rate capability of graphite can be improved, and meanwhile, Nb is added 2 O 5 And the lithium can be stored together with the graphite material to improve the reversible capacity of the lithium-ion battery.
Compared with the prior art, the invention has the following advantages:
1. the niobium pentoxide coated graphite composite negative electrode material has excellent cycling stability;
2. the graphite material is coated with niobium pentoxide and then sintered to form T-niobium pentoxide, so that the interface impedance can be effectively reduced, and the cycle stability and the rate capability of the T-niobium pentoxide can be improved;
3. the niobium pentoxide is uniformly coated on the surface of the graphite cathode by a simple and low-cost sol-gel method to form a uniformly distributed coating layer, and the method is simple, has low cost and can be used for large-scale production.
Drawings
FIG. 1 is an SEM image of a niobium pentoxide coated graphite composite anode material prepared in example 3 of the present invention;
FIG. 2 is an EDS diagram of a niobium pentoxide coated graphite composite anode material prepared in example 3 of the present invention;
FIG. 3 is an XRD pattern of a niobium pentoxide coated graphite composite negative electrode material prepared in example 3 of the present invention;
FIG. 4 is an XPS plot of a niobium pentoxide coated graphite composite anode material prepared in example 3 of the present invention;
FIG. 5 is an electrochemical impedance spectrum of a niobium pentoxide coated graphite composite anode material prepared in example 3 of the present invention;
FIG. 6 is a cyclic voltammetry curve of the niobium pentoxide coated graphite composite negative electrode material prepared in example 3 of the present invention at 0.01-3V;
FIG. 7 is a graph of capacity cycling of a half cell assembled with the niobium pentoxide coated graphite composite anode material prepared in example 3 of the present invention at a current density of 1C for 200 cycles;
FIG. 8 is a graph of the capacity cycling of 200 cycles of a Gr negative electrode material assembled half cell obtained in comparative example 1 at a current density of 1C;
FIG. 9 is a graph of capacity cycling of 1000 cycles of a half-cell assembled with the niobium pentoxide coated graphite composite anode material prepared in example 3 of the present invention at a current density of 10C;
FIG. 10 is a graph of capacity cycling of 1000 cycles of a half cell assembled with Gr negative electrode material obtained in comparative example 1 at a current density of 10C;
FIG. 11 is a graph showing the rate curves of half-cells assembled by the niobium pentoxide coated graphite composite negative electrode material prepared in example 3 under different current densities;
FIG. 12 is a graph of the rate of change of current density for half-cells assembled with Gr negative electrode material obtained in comparative example 1 of the present invention.
Detailed Description
The present invention will be described in detail with reference to the accompanying drawings and specific embodiments, and it is to be understood that the technical solutions in the embodiments of the present invention are described clearly and completely.
The niobium pentoxide-coated graphite composite negative electrode material comprises, by mass, 1-15 wt% of niobium pentoxide, wherein the niobium pentoxide forms uniformly distributed coating layers on the graphite negative electrode material, and the graphite negative electrode material is spherical particles of 5-15 μm.
Example 1
A) 0.10164g (0.00037621 mol) of niobium pentachloride (relative molecular mass 270.17) is weighed in a glove box and dissolved in 20mL of absolute ethyl alcohol, and the mixture is stirred for 0.5h at room temperature to form niobium alcohol solution;
B) dropwise adding 5ml of deionized water into the niobium alcohol solution prepared in the step A), stirring for 1h, and uniformly dispersing to form a mixed solvent;
C) adding 5g of graphite (the coating amount is 1wt% and is marked as Gr @ 1-Nb) into the mixed solvent prepared in the step B) 2 O 5 ) Stirring graphite in the form of spherical particles of 5-15 microns for 1h, uniformly dispersing, heating and stirring for 2h at 75 ℃ in a water bath at the stirring speed of 300r/min until the solvent is evaporated to dryness, drying in a 70 ℃ oven, and grinding into powder;
D) and C) sintering the powder prepared in the step C) in a tube furnace, and sintering for 2.5 hours in an argon atmosphere at the temperature rise rate of 5 ℃/min to 800 ℃ to obtain the niobium pentoxide coated graphite composite negative electrode material.
Example 2
A) 0.5082g (0.00188104 mol) of niobium pentachloride (relative molecular mass 270.17) is weighed in a glove box and dissolved in 20mL of absolute ethyl alcohol, and the mixture is stirred for 0.5h at room temperature to form niobium alcohol solution;
B) dropwise adding 5ml of deionized water into the niobium alcohol solution prepared in the step A), stirring for 1h, and uniformly dispersing to form a mixed solvent;
C) adding 5g of graphite (the coating amount is 5wt% and is marked as Gr @ 5-Nb) into the mixed solvent prepared in the step B) 2 O 5 ) Stirring graphite in the form of spherical particles of 5-15 microns for 1h, uniformly dispersing, heating and stirring for 2h at 70 ℃ in a water bath at the stirring speed of 400r/min until the solvent is evaporated to dryness, drying in a 50 ℃ oven, and grinding into powder;
D) and C) sintering the powder prepared in the step C) in a tube furnace, heating to 700 ℃ at a heating rate of 2 ℃/min in an argon atmosphere, and sintering for 3h to obtain the niobium pentoxide coated graphite composite negative electrode material.
Example 3
A) 1.0164g (0.00376208 mol) of niobium pentachloride (relative molecular mass 270.17) is weighed in a glove box and dissolved in 20mL of absolute ethyl alcohol, and the mixture is stirred for 0.5h at room temperature to form niobium alcohol solution;
B) dropwise adding 5ml of deionized water into the niobium alcohol solution prepared in the step A), stirring for 1h, and uniformly dispersing to form a mixed solvent;
C) adding 5g of graphite (the coating amount is 10wt% and is marked as Gr @ 10-Nb) into the mixed solvent prepared in the step B) 2 O 5 ) Stirring graphite in the form of spherical particles of 5-15 microns for 1h, uniformly dispersing, heating and stirring for 2h at the temperature of 80 ℃ in a water bath at the stirring speed of 600r/min until the solvent is evaporated to dryness, drying in an oven at the temperature of 80 ℃, and grinding into powder;
D) and C) sintering the powder prepared in the step C) in a tube furnace, heating to 800 ℃ at a heating rate of 10 ℃/min in an argon atmosphere, and sintering for 3h to obtain the niobium pentoxide coated graphite composite negative electrode material.
Example 4
A) 1.5246g (0.00564311 mol) of niobium pentachloride (relative molecular mass 270.17) is weighed in a glove box and dissolved in 20mL of absolute ethyl alcohol, and the mixture is stirred for 0.5h at room temperature to form niobium alcohol solution;
B) dropwise adding 5ml of deionized water into the niobium alcohol solution prepared in the step A), stirring for 1h, and uniformly dispersing to form a mixed solvent;
C) adding 5g of graphite (the coating amount is 15wt% and is marked as Gr @ 15-Nb) into the mixed solvent prepared in the step B) 2 O 5 ) Stirring graphite in the form of spherical particles of 5-15 microns for 1h, uniformly dispersing, heating and stirring for 2h at the temperature of 80 ℃ in a water bath at the stirring speed of 600r/min until the solvent is evaporated to dryness, drying in an oven at the temperature of 80 ℃, and grinding into powder;
D) sintering the powder prepared in the step D) in a tube furnace, heating to 900 ℃ at a heating rate of 10 ℃/min in an argon atmosphere, and sintering for 2h to obtain the niobium pentoxide coated graphite composite negative electrode material.
Comparative example 1
The anode material is a Gr anode material which is not coated with niobium pentoxide.
Taking example 3 as an example, the SEM of the obtained niobium pentoxide-coated graphite composite negative electrode material is shown in fig. 1, the particle size is about 10 μm, EDS is shown in fig. 2, niobium pentoxide is uniformly coated on the graphite surface, XRD is shown in fig. 3, which indicates that niobium pentoxide is T-niobium pentoxide with better rate capability, XPS is shown in fig. 4, and the niobium pentoxide-coated graphite composite negative electrode material has a peak of Nb.
The niobium pentoxide-coated graphite composite negative electrode material prepared in example 3 was assembled into a half cell by mixing the active material, acetylene black, sodium carboxymethylcellulose (CMC), and Styrene Butadiene Rubber (SBR) at 90: 5: 2: 3, then dispersing the mixture in deionized water with a magnetic stirrer for 6h to form a uniform slurry, then coating the slurry on a copper foil with a doctor blade, and finally drying in a vacuum oven at 120 ℃ for 12h to remove moisture. The electrode plate is manufactured by cutting a copper foil into a wafer with the diameter of 10mm, and the mass load of the cut electrode plate is 2.5-3.5 mg-cm -2 CR2016 coin cells were assembled in an argon glove box. A lithium metal sheet and a porous polypropylene film (Celgard 2400) were used as a counter electrode and a separator, respectively. The electrolyte adopts 1 mol.L dissolved in ethylene carbonate/ethyl methyl carbonate/dimethyl carbonate (EC/EMC/DMC) (volume ratio =1:1:1) -1 LiPF 6 。
As shown in fig. 5, the internal resistance of the half cell of the niobium pentoxide coated graphite composite negative electrode material prepared in this example 3 was greatly reduced. The cyclic voltammogram of the niobium pentoxide coated graphite composite negative electrode material of example 3 at 0.01-3V is shown in fig. 6, which clearly shows that there is an oxidation-reduction reaction of niobium pentoxide.
Fig. 7 is a graph showing a comparison of the capacity cycle of the half cell assembled with the niobium pentoxide-coated graphite composite anode material obtained in example 3 at 1C current density for 200 cycles, and fig. 8 is a graph showing the capacity cycle of the half cell assembled with the Gr anode material obtained in comparative example 1 at 1C current density for 200 cycles.
Under the condition of 0.01-3V and 1C, the first discharge specific capacity of the niobium pentoxide coated graphite composite negative electrode material is 373.5mAh/g, after 200 cycles, the capacity retention rate can reach 98.5%, and the capacity retention rate of unmodified graphite is only 53.3%.
Fig. 9 is a graph showing the capacity cycle of 1000 cycles of the half cell assembled with the niobium pentoxide-coated graphite composite anode material obtained in example 3 at a current density of 10C, and fig. 10 is a graph showing the capacity cycle of 1000 cycles of the half cell assembled with the Gr anode material obtained in comparative example 1 at a current density of 10C.
Under the conditions of 0.01-3V and 10C high rate, the niobium pentoxide coated graphite negative electrode material can still retain 70.6mAh/g of specific discharge capacity after being circulated for 1000 circles, and unmodified graphite only has 33.4mAh/g of specific discharge capacity.
Fig. 11 is a graph of the rate of charge of half cells assembled with the niobium pentoxide coated graphite anode material obtained in example 3 at different current densities, and fig. 12 is a graph of the rate of charge of half cells assembled with the Gr anode material obtained in comparative example 1 at different current densities, clearly showing that the niobium pentoxide coated graphite anode material has better fast charge performance.
According to the niobium pentoxide coated graphite composite negative electrode material and the preparation method thereof, the prepared niobium pentoxide coated graphite composite negative electrode material has excellent circulation stability, and the niobium pentoxide is coated on the graphite material and then sintered to form T-niobium pentoxide, so that the interface impedance can be effectively reduced, and the circulation stability and the rate capability of the material are improved; in addition, the niobium pentoxide is uniformly coated on the surface of the graphite cathode by a simple and low-cost sol-gel method to form uniformly distributed coating layers, and the method is simple, low in cost and capable of realizing large-scale production.
Here, it should be noted that the description of the above technical solutions is exemplary, the present specification may be embodied in different forms, and should not be construed as being limited to the technical solutions set forth herein. Rather, these descriptions are provided so that this disclosure will be thorough and complete, and will fully convey the scope of the disclosure to those skilled in the art. Furthermore, the technical solution of the present invention is limited only by the scope of the claims.
The disclosure is intended to describe aspects of the specification and claims only by way of example and, therefore, should not be limited to the details shown. In the above description, when a detailed description of related known functions or configurations is determined to unnecessarily obscure the focus of the present specification and claims, the detailed description will be omitted.
Where the terms "comprising", "having" and "including" are used in this specification, there may be another part or parts unless otherwise stated, and the terms used may generally be in the singular but may also be in the plural.
Finally, it should be noted that the above is a detailed description of the invention in conjunction with the specific embodiments, and the specific embodiments of the invention should not be considered as limited to these descriptions, and it should be understood that the invention is not limited to the specific embodiments, and that the invention is not limited to the embodiments described above. The above embodiments are merely representative examples of the present invention. It is obvious that the invention is not limited to the above-described embodiments, but that many variations are possible. Any simple modification, equivalent change and modification made to the above embodiments in accordance with the technical spirit of the present invention should be considered to be within the scope of the present invention.
Claims (6)
1. A niobium pentoxide coated graphite composite negative electrode material is characterized in that: the mass ratio of niobium pentoxide is 1-15 wt%, the niobium pentoxide forms a uniformly distributed coating layer on the graphite cathode material, and the graphite cathode material is spherical particles with the particle size of 5-15 mu m.
2. A method for preparing the niobium pentoxide coated graphite composite anode material according to claim 1, characterized in that: the method comprises the following steps:
A) dissolving niobium pentachloride in absolute ethyl alcohol to form a niobium alcohol solution;
B) dropwise adding deionized water into the niobium alcohol solution prepared in the step A), and uniformly stirring to form a mixed solvent;
C) adding graphite into the mixed solvent prepared in the step B) according to the molar ratio of niobium to graphite in the claim 1, uniformly stirring, evaporating the solvent to dryness in a water bath, putting the solvent into an oven for drying, and grinding the solvent into powder;
D) sintering the powder prepared in the step C) in a tubular furnace to obtain the niobium pentoxide coated graphite composite negative electrode material.
3. The method for preparing the niobium pentoxide coated graphite composite anode material as claimed in claim 2, wherein: in the step A), the solid-liquid mass ratio of the niobium alcohol solution is 1-15: 155.
4. the method for preparing the niobium pentoxide coated graphite composite anode material as claimed in claim 2, wherein: in the step B), in the mixed solvent, the ratio of the mass sum of the deionized water and the absolute ethyl alcohol to the mass of the niobium pentachloride is 205: (1-15).
5. The method for preparing the niobium pentoxide coated graphite composite anode material as claimed in claim 2, wherein: in the step C), the graphite is spherical particles of 5-15 microns, the temperature of a water bath is 70-80 ℃, the stirring speed in the water bath is 300-600 r/min until the solvent is evaporated to dryness, and the temperature of an oven is 50-80 ℃.
6. The method for preparing the niobium pentoxide coated graphite composite anode material as claimed in claim 2, wherein: in the step D), the sintering is carried out for 2-3 h in an argon atmosphere at a heating rate of 2-10 ℃/min to 700-900 ℃.
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