CN108269978B - Quantum dot/carbon tube sulfur-carrying composite cathode material and preparation method and application thereof - Google Patents
Quantum dot/carbon tube sulfur-carrying composite cathode material and preparation method and application thereof Download PDFInfo
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Abstract
The invention provides a quantum dot/carbon tube sulfur-carrying composite anode material and a preparation method and application thereof, and the technical scheme comprises the following steps: mixing and grinding carbon tube and sulfur, adding CS2Fully stirring and drying to obtain the carbon tube sulfur-carrying composite material; mixing the selenium (or sulfide) with carbon black and polyvinylidene fluoride according to a certain mass ratio, adding N-methyl pyrrolidone and selenium (or sulfide) quantum dots, stirring and ultrasonically dispersing uniformly, controlling the viscosity to be 1000-10000 cps to obtain slurry, coating the obtained slurry on a current collector aluminum foil in a thickness of 150-400 mm, and drying to obtain a selenium (or sulfide) quantum dot and carbon tube sulfur-carrying composite anode material; the preparation method of the selenium (or sulfide) compound quantum dot carbon tube composite anode material provided by the invention is simple to operate and easy for large-scale production; the prepared composite cathode material is used in the lithium-sulfur battery, can solve the problem that polysulfide ions are dissolved in liquid electrolyte in the charging and discharging processes of the lithium-sulfur battery, effectively inhibits the shuttle effect, and improves the coulombic efficiency and the cycling stability of the lithium-sulfur battery.
Description
Technical Field
The invention belongs to the field of nano composite material research, and particularly relates to a preparation method of a selenium (or sulfide) compound quantum dot/carbon tube composite positive electrode material for a lithium-sulfur battery in the aspects of improving the electrochemical performance of the lithium-sulfur battery, inhibiting polysulfide shuttle effect and the like.
Background
With the rapid development of economy and the increasing of energy consumption, the exhaustion of fossil fuel reserves and the environmental pollution caused by combustion make the demand of people for new alternative energy more and more urgent. The new energy, especially the chemical energy, has the characteristics of cleanness, environmental protection, safety, high efficiency and the like, and is favored by meeting the requirements of the strategy of sustainable development of human beings. Energy storage is a key of a plurality of innovative technologies, battery technology is greatly improved under the push of emerging concepts such as electric vehicles, batteries with various mechanisms are developed, but lithium-sulfur batteries are the most potential energy storage technology of the next generation. Since the commercialization of lithium ion batteries in 1991, through the development of more than 20 years, the performances of the positive and negative electrode materials of the conventional lithium ion batteries are close to the theoretical limit, but the lithium ion batteries still have unsatisfactory performance in terms of increasingly large energy storage systems. The lithium-sulfur battery has many advantages, and the theoretical specific capacity of the lithium-sulfur battery is 1675 mAh g-1It is 10 times of traditional lithium ion battery, and has rich sulfur storage, low cost, low toxicity and no public nuisance. However, lithium polysulfide formed in the lithium-sulfur battery during charging and discharging is easily dissolved in liquid electrolyte to cause shuttle effect, and volume expansion and corrosion of metal lithium during charging and discharging cause low utilization rate of active materials, low coulombic efficiency and poor cycle performance of the lithium-sulfur battery, which becomes an obstacle in the commercial application process of the lithium-sulfur battery.
In order to solve these problems and realize large-scale use of the lithium sulfur battery, research and development of a simple and low-cost preparation method are required to improve the electrochemical performance of the lithium sulfur battery, thereby improving the practical application prospect of the lithium sulfur battery.
Disclosure of Invention
The technical problem to be solved by the embodiment of the invention is to provide a preparation method of a quantum dot/carbon tube composite anode material, which is simple to operate, mild in condition and easy for large-scale production.
The second purpose of the invention is to provide a quantum dot/carbon tube composite anode material.
The third purpose of the invention is to provide an application of the quantum dot/carbon tube composite positive electrode material in the lithium-sulfur battery, which can solve the problem of dissolution of polysulfide ions in liquid electrolyte in the charging and discharging processes of the lithium-sulfur battery, effectively inhibit the shuttle effect, and improve the coulombic efficiency and the cycling stability of the lithium-sulfur battery.
In order to achieve the purpose, the invention adopts the following technical scheme:
a preparation method of a quantum dot/carbon tube sulfur-carried composite anode material comprises the following steps:
(1) preparing a carbon tube sulfur-carrying composite material:
mixing carbon tube and sulfur according to the ratio of 1:1-2, grinding uniformly, adding 3-6mLCS2Stirring the solution, and standing at room temperature to CS2After complete volatilization, preserving the heat of the residual substances in an oven at 120-160 ℃ for 8-12 h, and then cooling to room temperature to obtain the carbon tube sulfur-carrying composite material;
(2) preparing a quantum dot/carbon tube sulfur-loaded composite anode material:
mixing the carbon tube sulfur-loaded composite material obtained in the step (1), a conductive additive and a binder according to a ratio of 3-8:1:1, adding 2-5mL of N-methyl pyrrolidone and 1-20mg of a selenium or sulfide quantum dot reagent, stirring and ultrasonically dispersing uniformly, wherein the mass ratio of the addition amount of the selenium or sulfide quantum dot reagent to the carbon tube sulfur-loaded composite material is 1:20-200, controlling the viscosity to be 1000-10000 cps to obtain slurry, coating the obtained slurry on a current collector aluminum foil by using a scraper, and then transferring the aluminum foil to a drying oven at 40-60 ℃ to dry to obtain the selenium or sulfide quantum dot and carbon tube sulfur-loaded composite anode material.
Further setting is that the thickness of mass flow body aluminium foil be 30um, wash with N-methyl pyrrolidone and alcohol before the use to detach surface oxide layer and impurity, natural air-drying.
The conductive additive is carbon black, and the binder is polyvinylidene fluoride.
Further configured, in the step (2), the selenium or sulfide quantum dot reagent is a reagent having an adsorption capacity for polysulfide.
The invention also provides the application of the quantum dot/carbon tube sulfur-loaded composite cathode material as a cathode electrode of a lithium-sulfur battery.
The invention has the beneficial effects that:
(1) the selenium (or sulfide) quantum dots are adopted as the polysulfide adsorbent, so that the adsorption capacity is high;
(2) the prepared selenium (or sulfide) compound quantum dot and carbon tube sulfur-loaded composite anode material can additionally provide an electron/ion conduction path, reduce the internal resistance of the battery and greatly improve the discharge capacity and the cycle stability of the battery;
(3) the composite positive electrode material containing the selenium (or sulfide) quantum dots can enhance the reactivity with polysulfide and accelerate the chemical reaction kinetics, thereby inhibiting the shuttle effect and improving the performance of the lithium-sulfur battery;
(4) the carrier porous carbon provides a sulfur storage space and can limit the diffusion and transportation of polysulfide and lithium sulfide;
in summary, on the one hand, the invention provides a preparation method of the selenium (or sulfide) compound quantum dot carbon tube sulfur-carried composite anode material, which is simple to operate, does not involve high temperature and high pressure, can be completed at room temperature, and is easy for large-scale production; on the other hand, when the prepared composite cathode material is used in a lithium-sulfur battery, the problem that polysulfide ions are dissolved in liquid electrolyte in the charging and discharging processes of the lithium-sulfur battery can be solved, the shuttle effect is effectively inhibited, and the coulomb efficiency and the cycling stability of the lithium-sulfur battery are improved.
Drawings
Fig. 1 is a comparative graph of a charging and discharging platform of a lithium sulfur battery prepared by the selenide quantum dot and carbon tube sulfur-loaded composite cathode material in the embodiment 1 of the invention and the lithium sulfur battery without the selenide quantum dot material under 0.2C;
fig. 2 is a graph showing the comparison of the rate performance of the selenide quantum dot and carbon tube sulfur-loaded composite cathode material prepared in example 1 of the present invention for a lithium sulfur battery and a lithium sulfur battery without the selenide quantum dot material;
fig. 3 is a high surface density cycle performance diagram of the composite cathode material of sulfide quantum dots and carbon tube graphite prepared in example 2 of the present invention when used in a lithium-sulfur battery.
Detailed Description
The present invention is further illustrated by the following specific examples, but the scope of the present invention is not limited thereto.
Example 1
Preparation of selenide quantum dot and carbon tube sulfur-carried composite anode material and application in lithium-sulfur battery
(1) Preparing a carbon tube sulfur-carrying composite material: putting 200mg of carbon tube and 200mg of elemental sulfur into a mortar, fully and uniformly grinding porous carbon and sulfur, transferring the obtained mixture into a 25mL weighing bottle, and adding 3.2mL of CS2Stirring thoroughly until CS is obtained2Completely volatilizing, transferring the mixture to a 120 ℃ oven, preserving the temperature for 12h, then cooling to room temperature, and collecting the obtained product to obtain the carbon tube sulfur-carrying composite material;
(2) preparing a selenide quantum dot carbon tube sulfur-loaded composite anode material: 300mg of carbon tube sulfur-loaded composite material is mixed with 15mg of conductive additive carbon black, 15mg of adhesive polyvinylidene fluoride and 1mg of selenide quantum dots, then 2.5mL of NMP is added, ultrasonic dispersion and full stirring are carried out, the viscosity of slurry is controlled to be 10000cps, and then the slurry is coated on a current collector aluminum foil by a scraper with the thickness of 150mm (the aluminum foil is cleaned twice by NMP and alcohol to remove a surface oxide layer and impurities, and the aluminum foil is naturally air-dried, wherein the thickness of the aluminum foil is 30 um). Then transferring the aluminum foil into a drying oven at 40 ℃, and drying to obtain the required anode material;
(3) assembling the battery: cutting the composite electrode material prepared in the step (2) into round pieces with the diameter of 14mm, weighing the round pieces in a dry environment, andand deducting the mass of the blank aluminum sheet to prepare the positive pole piece for later use. As a comparison experiment, the carbon tube sulfur-carrying composite positive electrode material without selenide quantum dots is also prepared into a comparison positive electrode piece for standby by the same method; the cell assembly was carried out in a glove box filled with argon, water and oxygen, each less than lpm. Commercial lithium metal sheets were used as reference and counter electrodes, and LiTFSI/DOL.DMC (1: 1) was used with 1% LiNO dissolved3After a diaphragm of the liquid electrolyte is assembled into a CR2025 button cell by adopting Celgard2400, standing for 24 hours, and then carrying out charge and discharge tests;
(4) the Xinwei battery testing system performs battery charge and discharge tests under different multiplying powers, the testing conditions are room temperature environment, the window initial voltage is 1.5V, and the termination voltage is 3.0V;
fig. 1 is a comparison graph of a charging and discharging platform of the selenide quantum dot carbon tube sulfur-loaded composite cathode material prepared in the embodiment, which is used for a lithium sulfur battery, and a lithium sulfur battery without the selenide quantum dot added under 0.2C, and it can be seen from the graph that the capacity and the collection rate of the lithium sulfur battery with the carbon tube sulfur-loaded composite material with the selenide quantum dot are obviously superior to those of the lithium sulfur battery without the selenide quantum dot added.
Fig. 2 is a graph showing the comparison of rate performance of the selenide quantum dot carbon tube sulfur-loaded composite cathode material for a lithium sulfur battery and a lithium sulfur battery without the selenide quantum dot, and it is obvious from the graph that the lithium sulfur battery containing the selenide quantum dot cathode material has higher discharge capacity under various rates.
Example 2
Preparation of sulfide quantum dot and carbon tube sulfur-carried composite anode material and application of composite anode material in lithium-sulfur battery
(1) Preparing a carbon tube sulfur-carrying composite material: 200mg of the carbon tube composite material obtained above and 400mg of elemental sulfur are put into a mortar, porous carbon and sulfur are fully and uniformly ground, the obtained mixture is transferred into a 25mL weighing bottle, and 6mL of CS is added2Stirring thoroughly until CS is obtained2Completely volatilizing, transferring the mixture to a 150 ℃ oven, preserving the temperature for 10h, then cooling to room temperature, and collecting the obtained product to obtain the carbon tube sulfur-carrying composite material;
(2) preparing a sulfide quantum dot carbon tube sulfur-carrying composite anode material: mixing 400mg of the carbon tube sulfur-loaded composite material with 50mg of conductive additive carbon black, 50mg of adhesive polyvinylidene fluoride and 2mg of sulfide quantum dots, then adding 3.5mL of NMP, carrying out ultrasonic dispersion and full stirring, controlling the viscosity of slurry to be 6000cps, and then coating the slurry on a current collector aluminum foil by a scraper with the thickness of 150mm (the aluminum foil is cleaned twice by NMP and alcohol to remove a surface oxide layer and impurities, and is naturally air-dried, wherein the thickness of the aluminum foil is 30 um). Then transferring the aluminum foil into a 50 ℃ oven, and drying to obtain the required anode material;
(3) assembling the battery: and (3) cutting the composite electrode material prepared in the step (2) into round pieces with the diameter of 14mm, weighing in a dry environment, and deducting the mass of blank aluminum pieces to prepare a positive electrode piece for later use. As a contrast experiment, the carbon tube sulfur-carrying composite positive electrode material without sulfide quantum dots is also prepared into a contrast positive electrode piece for standby by the same method; the cell assembly was carried out in a glove box filled with argon, water and oxygen, each less than lpm. Commercial lithium metal sheets were used as reference and counter electrodes, and LiTFSI/DOL.DMC (1: 1) was used with 1% LiNO dissolved3After a diaphragm of the liquid electrolyte is assembled into a CR2025 button cell by adopting Celgard2400, standing for 24 hours, and then carrying out charge and discharge tests;
(4) the Xinwei battery testing system performs battery charge and discharge tests under different multiplying powers, the testing conditions are room temperature environment, the window initial voltage is 1.5V, and the termination voltage is 3.0V;
FIG. 3 shows that when the sulfide quantum dot carbon tube sulfur-carrying composite positive electrode material is used in a lithium-sulfur battery, the thickness of the composite positive electrode material is 3.6 mg/cm-2At a high areal density of (2), at 1.97mA · cm-2The current density of (a) was subjected to a cycle stability test, and it is understood from the figure that the battery containing sulfide quantum dots is excellent in both stability and capacity.
Claims (6)
1. A preparation method of a quantum dot/carbon tube sulfur-carried composite anode material is characterized by comprising the following steps:
(1) preparing a carbon tube sulfur-carrying composite material:
mixing carbon tube with sulfurMixing at a ratio of 1:1-2, grinding, adding 3-6mLCS2Stirring the solution, and standing at room temperature to CS2After complete volatilization, preserving the heat of the residual substances in an oven at 120-160 ℃ for 8-12 h, and then cooling to room temperature to obtain the carbon tube sulfur-carrying composite material;
(2) preparing a quantum dot/carbon tube sulfur-loaded composite anode material:
mixing the carbon tube sulfur-loaded composite material obtained in the step (1), a conductive additive and a binder according to a ratio of 3-8:1:1, adding 2-5mL of N-methyl pyrrolidone and 1-20mg of a selenide quantum dot reagent, stirring and ultrasonically dispersing uniformly, wherein the selenide quantum dot reagent is molybdenum selenide, the addition amount of the selenide quantum dot reagent is 1%, the viscosity is controlled to be 1000-10000 cps, obtaining slurry, coating the obtained slurry on a current collector aluminum foil by using a scraper, and transferring the aluminum foil to a drying oven at 40-60 ℃ for drying, so as to obtain the selenide quantum dot and carbon tube sulfur-loaded composite anode material.
2. The preparation method of claim 1, wherein the current collector aluminum foil has a thickness of 30 μm, is washed with N-methyl pyrrolidone and alcohol to remove a surface oxide layer and impurities before use, and is naturally air-dried.
3. The method of claim 1, wherein the conductive additive is carbon black and the binder is polyvinylidene fluoride.
4. The method according to claim 1, wherein in the step (2), the selenide quantum dot reagent is a reagent having an adsorption ability to polysulfide.
5. A quantum dot/carbon tube sulfur-carried composite anode material prepared by the preparation method of any one of claims 1 to 4.
6. The application of the quantum dot/carbon tube sulfur-loaded composite positive electrode material as claimed in claim 5 as a positive electrode in a lithium sulfur battery, characterized in that the quantum dot and the carbon tube sulfur-loaded composite positive electrode material are processed into the specification shape and the size of the positive electrode of the lithium sulfur battery as a positive electrode sheet.
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| CN109473640A (en) * | 2018-09-30 | 2019-03-15 | 温州大学 | Silicon substrate molecular sieve/carbon pipe carries sulphur composite positive pole and its preparation method and application |
| CN109494346B (en) * | 2018-10-25 | 2021-09-24 | 电子科技大学 | Preparation method of carbon quantum dot modified lithium-sulfur battery positive electrode material |
| CN109728297A (en) * | 2018-12-11 | 2019-05-07 | 温州大学 | Metal phthalocyanine/carbon pipe composite material preparation method and its application in lithium-sulphur cell positive electrode |
| CN109698331B (en) * | 2018-12-11 | 2021-04-23 | 温州大学 | Preparation method of sulfite/carbon tube sulfur-carrying composite positive electrode material in lithium-sulfur battery |
| CN109728267B (en) * | 2018-12-11 | 2021-09-07 | 温州大学 | Preparation method and application of composite material of phosphorus-containing micromolecule functionalized carbon nanotube |
| CN109755503B (en) * | 2018-12-13 | 2021-09-07 | 温州大学 | Preparation method of manganese compound/carbon tube sulfur-carrying composite material and application of manganese compound/carbon tube sulfur-carrying composite material in lithium-sulfur battery |
| CN109755504B (en) * | 2018-12-13 | 2021-09-07 | 温州大学 | Preparation method of ferriporphyrin/carbon nanotube composite positive electrode material and application of ferriporphyrin/carbon nanotube composite positive electrode material in positive electrode of lithium-sulfur battery |
| CN113410463B (en) * | 2021-06-03 | 2023-03-10 | 江苏智泰新能源科技有限公司 | Selenium metal compound-carbon material-sulfur composite cathode material, preparation method and application |
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