CN116154167A - Carbon-based composite positive electrode material of lithium-sulfur battery and preparation method thereof - Google Patents

Carbon-based composite positive electrode material of lithium-sulfur battery and preparation method thereof Download PDF

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CN116154167A
CN116154167A CN202211710356.5A CN202211710356A CN116154167A CN 116154167 A CN116154167 A CN 116154167A CN 202211710356 A CN202211710356 A CN 202211710356A CN 116154167 A CN116154167 A CN 116154167A
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lithium
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张炳森
戚聿杰
柴宁
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Institute of Metal Research of CAS
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Abstract

The invention discloses a carbon-based composite positive electrode material of a lithium-sulfur battery and a preparation method thereof, and belongs to the technical field of lithium-sulfur batteries. The method takes a hydrothermal carbonization product of sugar as a precursor, obtains a carbon-based matrix through high-temperature carbonization treatment, and adopts an impregnation method to load platinum nano particles on the surface layer of the matrix to prepare the carbon-based composite material. The method provided by the invention has the advantages of simple preparation process, controllable cost and good repeatability, and is suitable for large-scale production. The carbon-based composite positive electrode material prepared by the method has high specific surface area, relieves volume expansion in the charge and discharge process, promotes the conversion of lithium polysulfide, effectively inhibits the shuttle effect in the battery, and improves the cycle and the rate capability of the lithium-sulfur battery.

Description

Carbon-based composite positive electrode material of lithium-sulfur battery and preparation method thereof
Technical Field
The invention relates to the technical field of lithium sulfur batteries, in particular to a carbon-based composite positive electrode material of a lithium sulfur battery and a preparation method thereof.
Background
Lithium ion batteries play a key role in mobile devices (electric automobiles, unmanned aerial vehicles, smart phones, computers, etc.). However, the energy density of the traditional lithium ion battery system is limited (140-260 Wh kg -1 ) And has higher production cost (> $100 kW) -1 h -1 ) It is difficult to meet the increasingly developed demands of electronic devices, so that the development of novel high-energy electrochemical energy storage systems is imperative.
Theoretical specific capacity of lithium sulfur battery (1675 mAh g) -1 ) Specific gravity (2600 Wh kg) -1 ) All lead commercial lithium ion batteries by a wide margin, and is a novel energy storage system which is close to practical use and has great prospect. Over the years, lithium sulfur batteries have been limited by dendrite growth of metallic lithium, poor sulfur conductivity of the active species, the "shuttle effect" of lithium polysulfide, volume expansion, and the like. In the charge and discharge process, lithium polysulfide is accumulated in electrolyte near the positive electrode easily and is shuttled and diffused to the negative electrode under the action of concentration gradient and electric field, so that irreversible loss of active substance sulfur and massive consumption of the electrolyte are caused. Therefore, the shuttle effect problem is most prominent, and is a main bottleneck for affecting the actual energy density and the cycle life of the lithium-sulfur battery and restricting the industrialization process of the lithium-sulfur battery.
Researchers develop a great deal of researches around the shuttle effect inhibition, and at the present stage, strategies such as physical confinement, chemical adsorption, heterostructure compounding and the like are adopted to optimally design the lithium-sulfur battery anode material. However, the porous materials such as carbon nanotubes have limited restriction on lithium polysulfide, and have the problems of high electrolyte consumption and the like; the chemisorption strategy mostly adopts Nb 2 O 5 、VS 2 Transition metal compounds such as NV have problems such as poor conductivity and limited chemisorption capacity. Therefore, the novel positive electrode material is reasonably designed and constructed to inhibit the shuttle effect in the lithium-sulfur battery, improve the cycle performance of the lithium-sulfur battery, and is a powerful guarantee for the practicability and industrialization of the lithium-sulfur battery.
Disclosure of Invention
Aiming at the defects in the prior art, the invention aims to provide a carbon-based composite positive electrode material of a lithium-sulfur battery and a preparation method thereof, which aim to realize the rapid conversion of lithium polysulfide and the efficient inhibition of a shuttle effect and improve the energy density and the charge-discharge cycle performance of the positive electrode of the lithium-sulfur battery.
In order to achieve the above purpose, the technical scheme adopted by the invention is as follows:
the preparation method of the carbon-based composite cathode material of the lithium sulfur battery comprises the steps of taking a hydrothermal carbonization product of sugar as a precursor, obtaining a carbon-based matrix through high-temperature carbonization treatment, and loading platinum nano particles on the surface layer of the matrix by adopting an impregnation method to prepare the carbon-based composite material.
The method specifically comprises the following steps:
(1) Hydrothermal carbonization and high-temperature carbonization of sugar: sugar is dissolved in deionized water to prepare sugar solution with a certain molar ratio; placing the sugar solution into a hydrothermal reaction kettle, and reacting for 8-20 hours at the temperature of 160-200 ℃ to obtain a sugar polycondensation precursor; the obtained saccharide polycondensation precursor is placed in a tube furnace for high-temperature carbonization under the protection of inert gas, the carbonization temperature is 700-1000 ℃, the heating rate is 5 ℃/min, and the carbonization time is 30-240 min; carbonizing to obtain a carbon-based substrate;
(2) Preparation of platinum nanoparticles: preparing a glycol solution of platinum salt and a glycol solution of sodium hydroxide with certain concentration by adopting an alcohol reduction method and using glycol as a solvent and a reducing agent, uniformly mixing the glycol solution of platinum salt and the glycol solution of sodium hydroxide, and placing the obtained mixed solution in an oil bath pot at 160-200 ℃ in a nitrogen atmosphere for reflux stirring for 2-12 hours to prepare a colloidal solution of platinum nano particles;
(3) Preparation of carbon-based composite material: the platinum nano particles are loaded on a carbon-based matrix by adopting an impregnation method, and the method specifically comprises the following steps: weighing a proper amount of colloidal solution of the platinum nano particles, weighing 0.1-0.5 g of carbon-based matrix, adding a proper amount of ethanol, fully mixing, and stirring for 12 hours after ultrasonic vibration and uniform dispersion; carrying out suction filtration treatment on the obtained mixture, and placing a suction filtration product on a filter membrane in a 60 ℃ oven for drying for 12 hours to obtain a carbon-based composite material;
(4) Preparation of a positive electrode material: weighing a certain amount of carbon-based composite material and sublimed sulfur, grinding uniformly, then filling into a reaction kettle, and preserving heat for 12 hours at 155 ℃; grinding the obtained black solid, mixing with a conductive agent Super P, a binder PVDF and a solvent NMP according to a certain proportion, fully and uniformly stirring, coating the mixture on an aluminum foil, and vacuum drying at 60 ℃ for 12 hours to obtain the carbon-based composite anode material of the lithium-sulfur battery.
In the step (1), the sugar may be one of polysaccharide, disaccharide or monosaccharide.
In the step (1), the molar ratio of the sugar to the deionized water is 1: 50-1: 200.
in the step (2), the platinum salt is selected from one of chloroplatinic acid, platinum acetylacetonate, platinum tetrachloride and sodium chloroplatinate.
In the step (2), when the ethylene glycol solution of the platinum salt and the ethylene glycol solution of the sodium hydroxide are mixed, the molar ratio of the platinum salt to the sodium hydroxide is 1: 20-1: 100.
in the step (3), the loading of the platinum nano particles is 0.05 to 0.5 weight percent; and measuring the colloidal solution of the platinum nano particles according to the loading amount.
In the step (4), the mass ratio of the carbon-based composite material to the sublimed sulfur is (6-8): (2-4).
In the step (4), the mass ratio of the black solid, the conductive agent Super P and the binder PVDF is (7-9): (0.5-2): (0.5-1).
Compared with the prior art, the invention has the advantages and effects that:
1. the carbon-based material designed in the invention has low price and rich sources of raw materials, common sugar such as sucrose and glucose can be used as reaction raw materials, and the synthesis process is green, pollution-free and environment-friendly; and the composite anode material has simple whole preparation process and high repeatability, and is suitable for large-scale preparation and production.
2. The carbon-based substrate has high specific surface area, the surface layer contains a large number of nano-scale pore channels, sufficient limited space can be provided for lithium polysulfide, and the porous structure allows volume expansion in the charge and discharge process, so that the cycling stability of the battery is facilitated; meanwhile, the carbonization degree of the carbon-based matrix is high, so that the conductivity of the electrode material is ensured.
3. According to the invention, platinum nano particles are introduced as an electrocatalyst, so that the conversion process of intermediate product lithium polysulfide is accelerated, the shuttle effect in the charge and discharge process is effectively inhibited, the internal resistance of the battery can be effectively reduced, and the cycle and rate performance of the battery are improved; the loading of the platinum nano particles is several thousandths or even lower, the cost can be effectively controlled by the ultra-low loading, and the practicability of the electrode material is ensured.
4. The carbon-based composite positive electrode material prepared by the invention has relatively high cycle and multiplying power performance and outstanding comprehensive performance, and can be used as a positive electrode of a lithium-sulfur battery.
Drawings
FIG. 1 is an XRD pattern of a carbon-based matrix material according to the present invention;
FIG. 2 is an XRD pattern of a platinum-loaded nanoparticle carbon-based composite according to the present invention;
FIG. 3 is a graph showing the desorption and adsorption of nitrogen from a carbon-based matrix material according to the present invention;
FIG. 4 is a graph of nitrogen desorption adsorption of the platinum-loaded nanoparticle carbon-based composite of the present invention;
FIG. 5 is a graph showing pore size distribution of a carbon-based matrix material according to the present invention;
FIG. 6 is a graph of pore size distribution of a platinum-loaded nanoparticle carbon-based composite according to the present invention;
FIG. 7 is a graph showing the rate performance of the carbon-based matrix material according to the present invention;
FIG. 8 is a graph showing the rate performance of the carbon-based composite positive electrode material according to the present invention;
FIG. 9 is a graph showing the cycle performance of the carbon-based matrix material of the present invention at a current density of 0.2C;
fig. 10 is a graph showing the cycle performance of the carbon-based composite positive electrode material according to the present invention at a current density of 0.2C.
Detailed Description
The invention is described in further detail below with reference to specific examples and figures, which are intended to illustrate, but not to limit the invention.
The invention provides a preparation method of a carbon-based composite positive electrode material of a lithium-sulfur battery, which adopts a high-temperature carbonization method and an impregnation method to prepare the carbon-based composite material, and realizes the rapid conversion of lithium polysulfide and the effective inhibition of a shuttle effect.
Example 1:
(1) Hydrothermal carbonization and high-temperature carbonization of sugar: dissolving sucrose in deionized water to prepare a 0.5M sucrose solution, and placing the sucrose solution in a hydrothermal reaction kettle to react for 12 hours at the temperature of 180 ℃ to obtain a saccharide polycondensation precursor; and (3) placing the precursor into a tube furnace, and carbonizing at a high temperature under the protection of inert gas, wherein the carbonization temperature is 950 ℃, the heating rate is 5 ℃/min, and the carbonization time is 30min.
(2) Preparation of a positive electrode material: weighing a carbon-based substrate material and sublimed sulfur according to a mass ratio of 7:3, grinding uniformly, then filling into a reaction kettle, and preserving heat for 12 hours at 155 ℃; grinding the obtained black solid, mixing with a conductive agent Super P and a binder PVDF according to the mass ratio of 7:2:1, adding NMP, fully and uniformly stirring, coating to an aluminum foil, and vacuum drying at 60 ℃ for 12 hours to obtain the carbon-based body anode material.
The obtained carbon-based matrix material was characterized by an X-ray diffractometer (Rigaku D/MAX-2400), a specific surface area and porosity analyzer (trisar ii 3020), electrochemical performance measurements were performed on button cells assembled with the carbon-based matrix positive electrode material by using a new wiry cell test system (CT-4800), the XRD pattern of the carbon-based matrix material according to the present invention was shown in fig. 1, the nitrogen desorption adsorption curve of the carbon-based matrix material according to the present invention was shown in fig. 3, the pore size distribution curve of the carbon-based matrix material according to the present invention was shown in fig. 5, the rate performance curve of the carbon-based matrix material according to the present invention was shown in fig. 7, and the cycle performance at a current density of 0.2C was shown in fig. 9.
As can be seen from the graph, the graphitization degree of the carbon-based matrix material is higher, and the BET test result shows that the specific surface area is 340.7m 2 g -1 The surface layer contains a large number of holes; the electrochemical performance test results show that the discharge specific capacities of the carbon-based matrix positive electrode material at current densities of 0.1C, 0.2C, 0.5C, 1C and 2C are 678.9mAh g respectively -1 、571.3mAh g -1 、459.7mAh g -1 、339.6mAh g -1 、164.7mAh g -1 The specific capacity of the first-turn discharge at the current density of 0.2C is 520.8mAh g -1 The specific discharge capacity after 500 cycles is maintained at 187.5mAh g -1 The capacity fade rate per turn was 0.128%.
Example 2:
(1) Hydrothermal carbonization and high-temperature carbonization of sugar: dissolving sucrose in deionized water to prepare a 0.5M sucrose solution, and placing the sucrose solution in a hydrothermal reaction kettle to react for 12 hours at the temperature of 180 ℃ to obtain a saccharide polycondensation precursor; and (3) placing the precursor into a tube furnace, and carbonizing at a high temperature under the protection of inert gas, wherein the carbonization temperature is 950 ℃, the heating rate is 5 ℃/min, and the carbonization time is 30min.
(2) Preparation of platinum nanoparticles: alcohol reduction method is adopted, glycol is used as solvent and reducer, chloroplatinic acid is used as platinum salt, 0.135g hexa-water chloroplatinic acid is dissolved in 50ml glycol to prepare 0.005M ethylene glycol chloroplatinic acid solution, 0.3g sodium hydroxide is dissolved in 15ml glycol to prepare 0.5M sodium hydroxide glycol solution, the two solutions are uniformly mixed, and the mixture is placed in an oil bath pot at 160 ℃ under the protection of nitrogen to be refluxed and stirred for 4 hours, and 0.5mg ml is obtained after volume fixing -1 Is a colloidal solution of platinum nanoparticles.
(3) Preparation of carbon-based composite material: loading platinum nano particles to a carbon-based matrix by adopting an impregnation method, weighing 10ml of the colloidal solution, weighing 0.1g of the carbon-based matrix, adding 20ml of ethanol, fully mixing, uniformly dispersing by ultrasonic vibration, and stirring for 12 hours; and (3) carrying out suction filtration treatment on the mixed solution, and placing a suction filtration product on the filter membrane in a 60 ℃ oven for drying for 12 hours to obtain the carbon-based composite material.
(4) Preparation of a positive electrode material: weighing the carbon-based composite material and sublimed sulfur according to the mass ratio of 7:3, grinding uniformly, then filling into a reaction kettle, and preserving heat for 12 hours at 155 ℃; grinding the obtained black solid, mixing with a conductive agent Super P and a binder PVDF according to the mass ratio of 7:2:1, adding NMP, fully and uniformly stirring, coating to an aluminum foil, and vacuum drying at 60 ℃ for 12 hours to obtain the carbon-based composite anode material of the lithium-sulfur battery.
The obtained carbon-based composite material is characterized by an X-ray diffractometer (Rigaku D/MAX-2400), a specific surface area and porosity analyzer (TriStarII 3020), electrochemical performance measurement is carried out on a button cell assembled by the carbon-based composite positive electrode material by a new-wire cell testing system (CT-4800), an XRD pattern of the platinum-loaded nanoparticle carbon-based composite material is shown in FIG. 2, a nitrogen desorption adsorption curve chart of the platinum-loaded nanoparticle carbon-based composite material is shown in FIG. 4, a pore size distribution curve of the platinum-loaded nanoparticle carbon-based composite material is shown in FIG. 6, a multiplying power performance chart of the carbon-based composite positive electrode material is shown in FIG. 8, and a cycle performance chart of the carbon-based composite positive electrode material at a current density of 0.2C is shown in FIG. 10.
As can be seen from the graph, the graphitization degree of the carbon-based matrix material is higher, and the BET test result shows that the specific surface area is 274.3m 2 g -1 The surface layer contains a large number of holes; the electrochemical performance test results show that the discharge specific capacities of the carbon-based matrix positive electrode material at current densities of 0.1C, 0.2C, 0.5C, 1C and 2C are 991.9mAh g respectively -1 、772.2mAh g -1 、572.0mAh g -1 、472.1mAh g -1 、324.9mAh g -1 The specific capacity of the first-turn discharge at the current density of 0.2C is 900.4mAh g -1 The specific discharge capacity after 500 cycles is maintained at 355.1mAh g -1 The capacity fade rate per turn was 0.121%.
According to the embodiment, the carbon-based composite positive electrode material loaded with the electrocatalyst nano particles prepared by the method effectively inhibits the shuttle effect in the charge and discharge process, shows higher discharge capacity and good cycle stability, is simple and convenient in preparation process, controllable in cost, suitable for large-scale preparation and production, can be used as a positive electrode material of a lithium-sulfur battery, and can play a role in mobile equipment such as unmanned aerial vehicles, mobile phones and computers.
While the foregoing description illustrates and describes preferred embodiments of the present invention, it is to be understood that the invention is not limited to the forms disclosed herein, but is not to be construed as limited to other embodiments, and is capable of use in various other combinations, modifications and environments and is capable of changes or modifications within the spirit of the invention described herein, either as a result of the foregoing teachings or as a result of the knowledge or skill of the relevant art. And that modifications and variations which do not depart from the scope of the invention are intended to be within the scope of the invention as defined in the appended claims.

Claims (10)

1. A preparation method of a carbon-based composite positive electrode material of a lithium-sulfur battery is characterized by comprising the following steps: the method takes a hydrothermal carbonization product of sugar as a precursor, obtains a carbon-based matrix through high-temperature carbonization treatment, and adopts an impregnation method to load platinum nano particles on the surface layer of the matrix to prepare the carbon-based composite material.
2. The method for preparing the carbon-based composite positive electrode material of the lithium-sulfur battery, according to claim 1, is characterized in that: the method specifically comprises the following steps:
(1) Hydrothermal carbonization and high-temperature carbonization of sugar: sugar is dissolved in deionized water to prepare sugar solution with a certain molar ratio; placing the sugar solution into a hydrothermal reaction kettle, and reacting for 8-20 hours at the temperature of 160-200 ℃ to obtain a sugar polycondensation precursor; the obtained saccharide polycondensation precursor is placed in a tube furnace for high-temperature carbonization under the protection of inert gas, the carbonization temperature is 700-1000 ℃, the heating rate is 5 ℃/min, and the carbonization time is 30-240 min; carbonizing to obtain a carbon-based substrate;
(2) Preparation of platinum nanoparticles: preparing a glycol solution of platinum salt and a glycol solution of sodium hydroxide with certain concentration by adopting an alcohol reduction method and using glycol as a solvent and a reducing agent, uniformly mixing the glycol solution of platinum salt and the glycol solution of sodium hydroxide, and placing the obtained mixed solution in an oil bath pot at 160-200 ℃ in a nitrogen atmosphere for reflux stirring for 2-12 hours to prepare a colloidal solution of platinum nano particles;
(3) Preparation of carbon-based composite material: the platinum nano particles are loaded on a carbon-based matrix by adopting an impregnation method, and the method specifically comprises the following steps: weighing a proper amount of colloidal solution of the platinum nano particles, weighing 0.1-0.5 g of carbon-based matrix, adding a proper amount of ethanol, fully mixing, and stirring for 12 hours after ultrasonic vibration and uniform dispersion; carrying out suction filtration treatment on the obtained mixture, and placing a suction filtration product on a filter membrane in a 60 ℃ oven for drying for 12 hours to obtain a carbon-based composite material;
(4) Preparation of a positive electrode material: weighing a certain amount of carbon-based composite material and sublimed sulfur, grinding uniformly, then filling into a reaction kettle, and preserving heat for 12 hours at 155 ℃; grinding the obtained black solid, mixing with a conductive agent Super P, a binder PVDF and a solvent NMP according to a certain proportion, fully and uniformly stirring, coating the mixture on an aluminum foil, and vacuum drying at 60 ℃ for 12 hours to obtain the carbon-based composite anode material of the lithium-sulfur battery.
3. The method for preparing the carbon-based composite positive electrode material of the lithium-sulfur battery according to claim 2, which is characterized in that: in step (1), the sugar may be one of a polysaccharide, a disaccharide or a monosaccharide.
4. The method for preparing the carbon-based composite positive electrode material of the lithium-sulfur battery according to claim 2, which is characterized in that: in the step (1), the molar ratio of the sugar to the deionized water is 1: 50-1: 200.
5. the method for preparing the carbon-based composite positive electrode material of the lithium-sulfur battery according to claim 2, which is characterized in that: in the step (2), the platinum salt is selected from one of chloroplatinic acid, platinum acetylacetonate, platinum tetrachloride and sodium chloroplatinate.
6. The method for preparing the carbon-based composite positive electrode material of the lithium-sulfur battery according to claim 2, which is characterized in that: in the step (2), when the ethylene glycol solution of the platinum salt and the ethylene glycol solution of the sodium hydroxide are mixed, the molar ratio of the platinum salt to the sodium hydroxide is 1: 20-1: 100.
7. the method for preparing the carbon-based composite positive electrode material of the lithium-sulfur battery according to claim 2, which is characterized in that: in the step (3), the loading of the platinum nano particles is 0.05-0.5 wt%; and measuring the colloidal solution of the platinum nano particles according to the loading amount.
8. The method for preparing the carbon-based composite positive electrode material of the lithium-sulfur battery according to claim 2, which is characterized in that: in the step (4), the mass ratio of the carbon-based composite material to the sublimed sulfur is (6-8): (2-4).
9. The method for preparing the carbon-based composite positive electrode material of the lithium-sulfur battery according to claim 2, which is characterized in that: in the step (4), the mass ratio of the black solid, the conductive agent Super P and the binder PVDF is (7-9): (0.5-2): (0.5-1).
10. A lithium sulfur battery carbon-based composite cathode material prepared by the method of claims 1-9.
CN202211710356.5A 2022-12-29 2022-12-29 Carbon-based composite positive electrode material of lithium-sulfur battery and preparation method thereof Pending CN116154167A (en)

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