CN110534746B - Tungsten carbide/carbon nanotube composite material and preparation method and application thereof - Google Patents
Tungsten carbide/carbon nanotube composite material and preparation method and application thereof Download PDFInfo
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- CN110534746B CN110534746B CN201910886229.2A CN201910886229A CN110534746B CN 110534746 B CN110534746 B CN 110534746B CN 201910886229 A CN201910886229 A CN 201910886229A CN 110534746 B CN110534746 B CN 110534746B
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- H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
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Abstract
The invention belongs to the technical field of lithium-sulfur batteries, and particularly discloses a tungsten carbide/carbon nanotube composite material and a preparation method and application thereof. The preparation method comprises the following specific steps: uniformly dispersing the carboxylated carbon nano tube in water, adding a tungsten source, continuously and uniformly mixing, then adding a polyethyleneimine dispersing solution, continuously and uniformly stirring to obtain a mixed solution, and drying the mixed solution to obtain a solid sample, and calcining to obtain the tungsten carbide/carbon nano tube composite material. The method synthesizes the tungsten carbide with better crystallinity at the temperature of not higher than 1000 ℃, has economical operation, simple and convenient steps and easy realization; the tungsten carbide and the carbon nano tube are uniformly compounded, the synergistic effect of the tungsten carbide on the electric conductivity of polysulfide and the carbon nano tube is fully exerted, the shuttle of the polysulfide can be effectively limited, and the performance of the lithium-sulfur battery is improved.
Description
Technical Field
The invention belongs to the technical field of lithium-sulfur batteries, and particularly relates to a tungsten carbide/carbon nanotube composite material as well as a preparation method and application thereof.
Background
With the wide application of portable electronic products and new energy automobiles, energy storage materials with large capacity are urgently needed in the market, and the most commonly used lithium ion battery at present cannot meet the increasing requirement of endurance mileage. Lithium sulfur batteries are considered as powerful competitors for the next generation of energy storage devices due to their high theoretical specific capacity (1675mAh/g) and high specific energy (2600Wh/kg), but their large-scale commercial application still faces several major problems: (1) sulfur and discharge products (Li)2S/Li2S2) Insulation of (2); (2) the volume expansion in the discharging process easily causes the damage of the battery structure; (3) shuttle effect of soluble polysulfide intermediates. The shuttle effect is the passage of the discharged higher-order polysulphides through the separator by free diffusion and then into lower-order polysulphides and Li as a result of the acceptance of electrons at the negative electrode2S/Li2S2The process of (1). The polysulfide shuttle effect is the main cause of poor cycle performance of the batteryFor this reason.
In order to inhibit the shuttle effect of polysulphides, researchers have used different types of materials to prepare sulfur anodes. Carbon materials such as carbon nanotubes, carbon fibers, porous carbon spheres, and graphene have been widely studied because of their polysulfide adsorption ability and good electrical conductivity. However, the non-polarity of the carbon material results in weak binding force with the polysulfide, thereby limiting the performance of the corresponding lithium-sulfur battery. Transition metal oxides, including manganese dioxide, titanium dioxide and the like, are another choice of sulfur anode materials, and have strong acting force with polysulfide to well adsorb the polysulfide; then, the poor conductivity of the lithium-sulfur battery reduces the reaction kinetics, thereby hindering the improvement of the performance of the corresponding lithium-sulfur battery.
Disclosure of Invention
In order to overcome the disadvantages and shortcomings of the prior art, the invention provides a method for preparing a tungsten carbide/carbon nanotube composite material.
The invention also aims to provide the tungsten carbide/carbon nano tube composite material prepared by the method.
The invention further aims to provide application of the tungsten carbide/carbon nanotube composite material in a lithium-sulfur battery.
The purpose of the invention is realized by the following scheme:
a preparation method of a tungsten carbide/carbon nanotube composite material comprises the following specific steps:
uniformly dispersing the carboxylated carbon nano tube in water, adding a tungsten source, continuously and uniformly mixing, then adding a polyethyleneimine dispersing solution, continuously and uniformly stirring to obtain a mixed solution, and drying the mixed solution to obtain a solid sample, and calcining to obtain the tungsten carbide/carbon nano tube composite material.
The mass volume ratio of the carboxylated carbon nanotubes to water is 0.1-0.5 g: 25 mL;
the tungsten source includes, but is not limited to, at least one of tungsten hexachloride and sodium tungstate;
the mass fraction of polyethyleneimine in the polyethyleneimine dispersion liquid is 1-100 g/L.
The mass-volume ratio of the carboxylated carbon nanotube to the tungsten source to the polyethyleneimine dispersion liquid is 0.1-0.5 g: 0.05-0.1 g: 2 mL;
the calcination is carried out in an atmosphere furnace, the calcination temperature is 800-1000 ℃, and the heating rate is 2-10 ℃ per minute; the calcination time is 1-2 h. The calcination is preferably carried out under an inert gas and nitrogen.
A tungsten carbide/carbon nano tube composite material obtained by the method.
The tungsten carbide/carbon nano tube composite material is applied to a lithium-sulfur battery.
A lithium-sulfur battery positive electrode prepared from the tungsten carbide/carbon nanotube composite material is prepared by the following steps:
grinding the tungsten carbide/carbon nano tube composite material and sublimed sulfur, and then placing the ground tungsten carbide/carbon nano tube composite material and sublimed sulfur in an inert atmosphere for heating reaction to obtain a tungsten carbide/carbon nano tube-sulfur composite material; and then fully mixing the tungsten carbide/carbon nanotube-sulfur composite material with a conductive agent and a binder, dispersing the mixture in a solvent, grinding the mixture into slurry, uniformly coating the slurry on an aluminum foil, and drying the aluminum foil to obtain the lithium-sulfur battery anode.
The mass ratio of the tungsten carbide/carbon nanotube composite material to the sublimed sulfur is 1: 1-1: 9;
the mass fraction of sulfur in the tungsten carbide/carbon nanotube-sulfur composite material is 50-90%.
The heating reaction is carried out for 1-24 h at 100-300 ℃; preferably at 155 ℃ for 6 h.
The conductive agent is at least one of Super P, Ketjen black and acetylene black; the binder is at least one of polyvinylidene fluoride, gelatin and sodium alginate; the solvent is at least one of N-methyl pyrrolidone and water.
The mass ratio of the tungsten carbide/carbon nanotube-sulfur composite material to the conductive agent to the binder is 6-9: 2-0.5: 2 to 0.5; preferably 8:1
The solvent is 0.5-5 mL for each 1g of the tungsten carbide/carbon nanotube-sulfur composite material.
Compared with the prior art, the invention has the following advantages and beneficial effects:
the method synthesizes the tungsten carbide with better crystallinity at the temperature of not higher than 1000 ℃, has economical operation, simple and convenient steps and easy realization; the tungsten carbide and the carbon nano tube are uniformly compounded, the synergistic effect of the tungsten carbide on the electric conductivity of polysulfide and the carbon nano tube is fully exerted, the shuttle of the polysulfide can be effectively limited, and the performance of the lithium-sulfur battery is improved.
Drawings
Fig. 1 is an XRD pattern of the tungsten carbide/carbon nanotube composite synthesized in example 1.
Fig. 2 is a graph showing cycle performance of the lithium sulfur batteries obtained in example 1 and comparative example 1.
Fig. 3 is a graph showing cycle performance of the lithium sulfur batteries obtained in example 2 and comparative example 1.
Detailed Description
The present invention will be described in further detail with reference to examples and drawings, but the embodiments of the present invention are not limited thereto.
The reagents used in the examples are commercially available without specific reference.
Carboxylated carbon nanotubes were purchased from alatin (C139960); polyvinylidene fluoride is commercially available from suwei (Solef 5130).
Example 1
Preparing a tungsten carbide/carbon nano tube composite material: weighing 0.1g of carboxylated carbon nanotubes, placing the carboxylated carbon nanotubes in a beaker, adding 25mL of water, and carrying out ultrasonic treatment for 20 minutes to uniformly disperse the carbon nanotubes in a solvent; adding 0.05g of sodium tungstate under vigorous stirring, and continuing stirring for 30 minutes; slowly adding 2mL of polyethyleneimine water dispersion with the concentration of 50g/L, stirring for 30 minutes, and then centrifugally drying to obtain a solid sample; and grinding the obtained sample, and calcining the ground sample at 900 ℃ for 2 hours at the heating rate of 5 ℃/min in the nitrogen atmosphere to obtain the tungsten carbide/carbon nano tube composite material.
Preparing a positive electrode: taking a certain amount of tungsten carbide/carbon nano tube composite material, fully grinding the tungsten carbide/carbon nano tube composite material with sublimed sulfur according to the proportion of 3:7, and then heating the mixture for 6 hours at the temperature of 155 ℃ in inert atmosphere to obtain the tungsten carbide/carbon nano tube-sulfur composite material. The materials are fully mixed with Super P and polyvinylidene fluoride according to the ratio of 8:1:1, then the mixture is dispersed in N-methyl pyrrolidone to be prepared into slurry, 2mL of N-methyl pyrrolidone is correspondingly added into each gram of tungsten carbide/carbon nano tube composite material, the mixture is uniformly coated on an aluminum foil, and the aluminum foil is dried to obtain the lithium-sulfur battery anode which is then used for preparing a lithium-sulfur battery (sample 2).
Example 2
Preparing a tungsten carbide/carbon nano tube composite material: weighing 0.5g of carboxylated carbon nanotubes, placing the carboxylated carbon nanotubes in a beaker, adding 25mL of water, and carrying out ultrasonic treatment for 20 minutes to uniformly disperse the carbon nanotubes in a solvent; adding 0.1g of tungsten hexachloride under vigorous stirring, and continuing stirring for 30 minutes; slowly adding 2mL of polyethyleneimine ethanol dispersion with the concentration of 100g/L, stirring for 30 minutes, and centrifugally drying to obtain a solid sample; and grinding the obtained sample, and calcining the ground sample at 900 ℃ for 2 hours at the heating rate of 2 ℃/min in the nitrogen atmosphere to obtain the tungsten carbide/carbon nanotube composite material.
Preparing a positive electrode: taking a certain amount of tungsten carbide/carbon nano tube composite material, fully grinding the tungsten carbide/carbon nano tube composite material with sublimed sulfur according to the proportion of 2:8, and then heating the mixture for 6 hours at 155 ℃ in an inert atmosphere to obtain the tungsten carbide/carbon nano tube-sulfur composite material. The materials are fully mixed with Super P and polyvinylidene fluoride according to the ratio of 8:1:1, then the mixture is dispersed in N-methyl pyrrolidone to be prepared into slurry, 4mL of N-methyl pyrrolidone is correspondingly added to each gram of tungsten carbide/carbon nano tube composite material, the slurry is uniformly coated on an aluminum foil, and the aluminum foil is dried to obtain the lithium-sulfur battery anode which is then used for preparing the lithium-sulfur battery. (sample 2)
Comparative example 1
Taking a certain amount of carbon nano tubes, fully grinding the carbon nano tubes and sublimed sulfur according to the proportion of 3:7, and then placing the carbon nano tubes and the sublimed sulfur in an inert atmosphere for heating at 155 ℃ for 6 hours to obtain the carbon nano tube-sulfur composite material. The materials are fully mixed with Super P and polyvinylidene fluoride according to the ratio of 8:1:1, then dispersed in N-methyl pyrrolidone to be prepared into slurry, 2mL of N-methyl pyrrolidone is correspondingly added into each gram of carbon nano tube, the mixture is uniformly coated on an aluminum foil, and the aluminum foil is dried to obtain the lithium-sulfur battery anode which is then used for preparing the lithium-sulfur battery (sample 1).
Fig. 1 is an XRD pattern of the tungsten carbide/carbon nanotube composite synthesized in example 1, from which it can be seen that the tungsten carbide/carbon nanotube composite was successfully synthesized, in which the crystallinity of the tungsten carbide component was good. Fig. 2 shows cycle performance of the lithium sulfur batteries obtained in example 1 and comparative example 1. Wherein the first-turn discharge capacity of the lithium-sulfur battery of the sample 2 obtained in the example 1 reaches 1263mAh/g, and the specific capacity of the lithium-sulfur battery still reaches 929mAh/g after 0.5C rotation, which is obviously better than that of the lithium-sulfur battery (sample 1) obtained in the comparative example 1.
Fig. 3 is a graph showing the performance of a lithium sulfur battery using the tungsten carbide/carbon nanotube composite material prepared in example 2 as a positive electrode material. Wherein the first-turn discharge capacity of the lithium-sulfur battery of the sample 2 obtained in the example 2 reaches 1381mAh/g, and the specific capacity of the lithium-sulfur battery after 0.5C rotation still reaches 1053mAh/g, which is obviously superior to the lithium-sulfur battery (sample 1) obtained in the comparative example 1.
The above embodiments are preferred embodiments of the present invention, but the present invention is not limited to the above embodiments, and any other changes, modifications, substitutions, combinations, and simplifications which do not depart from the spirit and principle of the present invention should be construed as equivalents thereof, and all such changes, modifications, substitutions, combinations, and simplifications are intended to be included in the scope of the present invention.
Claims (9)
1. A preparation method of a tungsten carbide/carbon nanotube composite material is characterized by comprising the following specific steps:
uniformly dispersing the carboxylated carbon nanotubes in water, adding a tungsten source, continuously and uniformly mixing, then adding a polyethyleneimine dispersing solution, continuously and uniformly stirring to obtain a mixed solution, drying the mixed solution to obtain a solid sample, and calcining to obtain the tungsten carbide/carbon nanotube composite material;
the calcination is carried out in an atmosphere furnace, the calcination temperature is 800-1000 ℃, and the heating rate is 2-10 ℃ per minute; the calcination time is 1-2 h.
2. The method for preparing a tungsten carbide/carbon nanotube composite material according to claim 1, characterized in that:
the mass-volume ratio of the carboxylated carbon nanotube to the tungsten source to the polyethyleneimine dispersion liquid is 0.1-0.5 g: 0.05-0.1 g: 2 mL.
3. The method for preparing a tungsten carbide/carbon nanotube composite material according to claim 1, characterized in that:
the mass volume ratio of the carboxylated carbon nanotubes to water is 0.1-0.5 g: 25 mL;
the mass fraction of polyethyleneimine in the polyethyleneimine dispersion liquid is 1-100 g/L;
the tungsten source includes at least one of tungsten hexachloride and sodium tungstate.
4. The tungsten carbide/carbon nanotube composite material prepared by the method according to any one of claims 1 to 3.
5. Use of the tungsten carbide/carbon nanotube composite material of claim 4 in a lithium sulfur battery.
6. A lithium-sulfur battery positive electrode prepared from the tungsten carbide/carbon nanotube composite material of claim 4, which is characterized by being prepared by the following method:
grinding the tungsten carbide/carbon nano tube composite material and sublimed sulfur, and then placing the ground tungsten carbide/carbon nano tube composite material and sublimed sulfur in an inert atmosphere for heating reaction to obtain a tungsten carbide/carbon nano tube-sulfur composite material; and then fully mixing the tungsten carbide/carbon nanotube-sulfur composite material with a conductive agent and a binder, dispersing the mixture in a solvent, grinding the mixture into slurry, uniformly coating the slurry on an aluminum foil, and drying the aluminum foil to obtain the lithium-sulfur battery anode.
7. The positive electrode of the lithium-sulfur battery prepared from the tungsten carbide/carbon nanotube composite material of claim 6, wherein: the mass ratio of the tungsten carbide/carbon nanotube composite material to the sublimed sulfur is 1: 1-1: 9.
8. The positive electrode of the lithium-sulfur battery prepared from the tungsten carbide/carbon nanotube composite material of claim 6, wherein:
the heating reaction is carried out for 1-24 h at 100-300 ℃;
the conductive agent is at least one of Super P, Ketjen black and acetylene black; the binder is at least one of polyvinylidene fluoride, gelatin and sodium alginate; the solvent is at least one of N-methyl pyrrolidone and water.
9. The positive electrode of the lithium-sulfur battery prepared from the tungsten carbide/carbon nanotube composite material of claim 6, wherein:
the mass ratio of the tungsten carbide/carbon nanotube-sulfur composite material to the conductive agent to the binder is 6-9: 2-0.5: 2 to 0.5;
the solvent is 0.5-5 mL for each 1g of the tungsten carbide/carbon nanotube-sulfur composite material.
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