CN112599740A - Tin disulfide/carbon cathode composite material for lithium ion battery and preparation method and application thereof - Google Patents
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Abstract
The invention discloses a tin disulfide/carbon cathode composite material for a lithium ion battery and a preparation method and application thereof, belonging to the field of lithium ion battery materials. The method comprises the following steps: (1) putting tin-containing compound powder into a tubular furnace, carrying out high-temperature pyrolysis reaction under protective atmosphere, and cleaning an obtained sample with deionized water to obtain a tin-carbon composite material; (2) dissolving the tin-carbon composite material in deionized water, and performing ultrasonic dispersion to obtain a solution A; (3) adding thiourea into the solution A obtained in the step (2), and stirring to obtain a solution B; (4) transferring the obtained solution B into a reaction kettle, carrying out hydrothermal reaction, and naturally cooling to room temperature after the reaction is finished to obtain a precipitate C; (5) and (4) centrifugally washing the precipitate C by using deionized water and absolute ethyl alcohol in sequence, and drying in a vacuum drying oven to obtain the tin disulfide/carbon composite material. The method has simple process, low cost, large-scale synthesis and high yield.
Description
Technical Field
The invention relates to a preparation method of a lithium ion battery cathode material, in particular to a tin disulfide/carbon cathode composite material of a lithium ion battery and a preparation method and application thereof, belonging to the field of lithium ion battery materials.
Background
Today, the problem of environmental pollution is receiving a lot of attention due to the large-scale use of fossil energy, and people are gradually inclined to use clean and pollution-free energy in order to delay or even prevent the progress of environmental degradation, while lithium ion batteries are a good choice. The lithium ion battery has the advantages of good cycle performance, high energy density, no memory effect, environmental protection and the like, and successfully replaces the traditional lead-acid storage battery and is commercialized. Commercial graphite cathodes can only provide 372mAh/g specific capacity, which requires that we look for high performance cathode materials to meet the increasing energy demand of human beings. At present, tin-based materials are greatly concerned due to higher theoretical specific capacity, wherein the layered tin disulfide material is considered to be one of the most promising negative electrode materials due to the unique CdI2 layered hexagonal structure which is favorable for the intercalation and deintercalation of lithium. However, the large volume expansion and low conductivity are two key issues limiting their practical application.
Typically, tin disulfide is composited with carbon materials to mitigate volume expansion and improve electrical conductivity. For example, CN107394129A discloses a method for preparing a tin disulfide-carbon nanotube composite electrode material, in which thioacetamide, tin tetrachloride pentahydrate, and multi-walled carbon nanotubes are used as a sulfur source, a tin source, and a carbon source, respectively, to prepare a tin disulfide-carbon nanotube composite material (liuhui, danluo, etc. [ P) by a hydrothermal method]). Recently, Wu et al prepared the ternary compound SnS by hydrothermal and low-temperature chemical vapor deposition techniques using thiourea, tin tetrachloride pentahydrate and reduced graphene oxide as a sulfur source, a tin source and a carbon source, respectively2/C-rGO(Y.-Q.Wu,Y.-S.Zhao,W.-J.Meng,et al.Nanoplates-assembled SnS2nanoflowers with can isolated coated on reduced graphene oxide for high performance Li-ion batteries, applied Surface Science,2021,539, 148283-. At present, a tin disulfide/carbon composite material is mainly synthesized by a hydrothermal method, and in the preparation process, a tin source and a carbon source are added into a solvent by two different substances, and the sources of the two substances are also different. Such a preparation process is relatively complicated, greatly increases the cost of raw materials, and is not favorable for large-scale production. Therefore, the composite material of the tin source and the carbon source from the same substance is synthesized, the raw material cost can be reduced, and the preparation process is simplified, which has important significance for industrial production.
Disclosure of Invention
The invention aims to provide a preparation method of a tin disulfide/carbon cathode composite material of a lithium ion battery, which is simple in preparation process.
The invention is realized by the following technical scheme:
a preparation method of a tin disulfide/carbon composite material comprises the following steps:
(1) putting a tin-containing compound into a tubular furnace, carrying out high-temperature pyrolysis reaction in a protective atmosphere, heating to a certain temperature in the tubular furnace, preserving the temperature for a period of time, naturally cooling to room temperature after the reaction is finished, and cleaning an obtained sample with water to obtain the tin-carbon composite material;
(2) dissolving a certain amount of tin-carbon composite material in water, and performing ultrasonic dispersion to obtain a solution A;
(3) adding a certain amount of thiourea into the solution A obtained in the step (2), and stirring to obtain a solution B;
(4) transferring the solution B obtained in the step (3) to a reaction kettle, carrying out hydrothermal reaction, and naturally cooling to room temperature after the reaction is finished to obtain a precipitate C;
(5) and (4) carrying out centrifugal washing on the precipitate C obtained in the step (4) by using water and absolute ethyl alcohol in sequence, and then placing the precipitate C in a vacuum drying oven for drying to obtain the tin disulfide/carbon composite material.
Preferably, the tin-containing compound in step (1) comprises one, two or more of dimethyltin oxide, dimethyltin dichloride, disodium stannous citrate, tributyltin oxide, butyltin trichloride, trichloromethyltin and tributyltin chloride; when the tin-containing compound is three, the molar ratio of any three tin-containing compounds is 1: (0-2.5): (0 to 3.0).
Preferably, the protective atmosphere in the step (1) comprises argon, nitrogen or a mixed gas of argon and hydrogen, and the volume ratio of argon to hydrogen in the mixed gas is (9-19): 1.
Preferably, the reaction temperature of the pyrolysis reaction in the step (1) is 500-1200 ℃, the heating rate is 2-20 ℃/min, and the heat preservation time is 0.5-8 h; the cleaning water is deionized water, and the temperature is 20-90 ℃.
Preferably, the mass concentration of the tin-carbon composite material in the step (2) in water is 0.125-0.5 mol/L; and (3) the time of ultrasonic dispersion in the step (2) is 0.5-2 h.
Preferably, the molar ratio of the thiourea in the step (3) to the sulfur element and the tin element in the tin-carbon composite material in the step (2) is (1-4): 1; and (4) stirring for 1-3 h in the step (3).
Preferably, the temperature of the hydrothermal reaction in the step (4) is 160-200 ℃, and the reaction time is 8-24 h.
Preferably, the drying temperature in the step (5) is 60-90 ℃.
The invention also provides the tin disulfide/carbon composite material prepared by the preparation method.
The invention also provides application of the tin disulfide/carbon composite material in preparation of a lithium ion battery cathode.
The invention has the following characteristics and advantages: the preparation method is simple, is suitable for large-scale production, directly prepares the tin-carbon composite material by using a one-step method, has no pollution, does not need to add any chemical reagent, directly carries out hydrothermal reaction with thiourea, is convenient to operate, has low energy consumption and has industrial prospect.
Drawings
Figure 1 is an XRD pattern of the tin disulfide/carbon composite prepared by the method of example 1.
FIG. 2 is a plot of the cycle discharge capacity at 100mA/g for the lithium ion battery prepared in example 1.
Detailed Description
The following non-limiting examples are presented to enable those of ordinary skill in the art to more fully understand the present invention and are not intended to limit the invention in any way.
The test methods described in the following examples are all conventional methods unless otherwise specified; the materials are commercially available, unless otherwise specified.
Example 1
A preparation method of a tin disulfide/carbon composite negative electrode material of a lithium ion battery comprises the following steps:
(1) and (2) mixing dimethyltin dichloride and trichloromethyltin according to the molar ratio of 1:0.45, putting the mixture into a tube furnace, calcining the mixture for 1h at 750 ℃ under the argon atmosphere at the heating rate of 10 ℃/min, taking out a sample after the temperature of the tube furnace is naturally cooled to the room temperature, and cleaning the sample with deionized water at 40 ℃ to obtain the tin-carbon composite material.
(2) Weighing 1.4875g of tin-carbon composite material, dissolving in 20mL of deionized water, and performing ultrasonic dispersion for 0.5h to obtain a solution A;
(3) weighing 0.76g of thiourea, adding the thiourea into the solution A obtained in the step (2), and stirring for 1h to obtain a solution B;
(4) transferring the solution B obtained in the step (3) into a reaction kettle, carrying out hydrothermal reaction for 8h at 160 ℃, and naturally cooling to room temperature after the reaction is finished to obtain a precipitate C;
(5) and (4) carrying out centrifugal washing on the precipitate C obtained in the step (4) by using deionized water and absolute ethyl alcohol in sequence, and then placing the precipitate C in a vacuum drying oven at 70 ℃ for drying for 10 hours to obtain the tin disulfide/carbon composite material.
X-ray diffraction analysis showed that the tin disulfide/carbon composite was made with a tin disulfide phase and amorphous carbon composition, see figure 1.
Taking the prepared tin disulfide/carbon composite material as a negative active material, mixing the prepared tin disulfide/carbon composite material with acetylene black and polyvinylidene fluoride in a proportion of 80: 10: 10, adding the mixture into an N-methyl pyrrolidone solvent, and uniformly mixing; coating the copper foil with the thickness of 20 microns on the copper foil, placing the copper foil in a vacuum oven to dry for 10 hours at the temperature of 80 ℃, and taking out the copper foil to prepare a lithium ion battery negative pole piece for testing; the cathode plate, the anode plate made of the ternary cathode material and the diaphragm form a lithium ion full battery, and the test result is shown in figure 2, and the result shows that the tin disulfide/carbon composite cathode material has good performance.
Example 2
A preparation method of a tin disulfide/carbon composite negative electrode material of a lithium ion battery comprises the following steps:
(1) mixing butyltin trichloride and dimethyltin oxide according to a molar ratio of 1:1.95, putting the mixture into a tubular furnace, calcining the mixture for 2 hours at 850 ℃ under a nitrogen atmosphere, heating at a rate of 8 ℃/min, taking out a sample after the temperature of the tubular furnace is naturally cooled to room temperature, and cleaning the sample with deionized water at 50 ℃ to obtain the tin-carbon composite material.
(2) Weighing 1.4875g of tin-carbon composite material, dissolving in 60mL of deionized water, and performing ultrasonic dispersion for 1h to obtain a solution A;
(3) weighing 1.52g of thiourea, adding the thiourea into the solution A obtained in the step (2), and stirring for 2 hours to obtain a solution B;
(4) transferring the solution B obtained in the step (3) into a reaction kettle, carrying out hydrothermal reaction at 170 ℃ for 12h, and naturally cooling to room temperature after the reaction is finished to obtain a precipitate C;
(5) and (4) carrying out centrifugal washing on the precipitate C obtained in the step (4) by using deionized water and absolute ethyl alcohol in sequence, and then placing the precipitate C in a vacuum drying oven at 80 ℃ for drying for 12 hours to obtain the tin disulfide/carbon composite material.
Example 3
A preparation method of a tin disulfide/carbon composite negative electrode material of a lithium ion battery comprises the following steps:
(1) and (2) putting the disodium stannous citrate into a tube furnace, calcining for 1h at 800 ℃ in a nitrogen atmosphere at the heating rate of 6 ℃/min, naturally cooling the tube furnace to room temperature, taking out a sample, and cleaning with deionized water at 60 ℃ to obtain the tin-carbon composite material.
(2) Weighing 1.4875g of tin-carbon composite material, dissolving in 40mL of deionized water, and performing ultrasonic dispersion for 1h to obtain a solution A;
(3) weighing 2.28g of thiourea, adding the thiourea into the solution A obtained in the step (2), and stirring for 0.5h to obtain a solution B;
(4) transferring the solution B obtained in the step (3) into a reaction kettle, carrying out hydrothermal reaction at 180 ℃ for 16h, and naturally cooling to room temperature after the reaction is finished to obtain a precipitate C;
(5) and (4) carrying out centrifugal washing on the precipitate C obtained in the step (4) by using deionized water and absolute ethyl alcohol in sequence, and then placing the precipitate C in a vacuum drying oven at 90 ℃ for drying for 14h to obtain the tin disulfide/carbon composite material.
Example 4
A preparation method of a tin disulfide/carbon composite negative electrode material of a lithium ion battery comprises the following steps:
(1) and (2) putting the dimethyl tin oxide into a tube furnace, calcining for 3h at 650 ℃ under the argon atmosphere, heating at the rate of 4 ℃/min, naturally cooling the tube furnace to room temperature, taking out a sample, and cleaning with deionized water at 30 ℃ to obtain the tin-carbon composite material.
(2) Weighing 1.4875g of tin-carbon composite material, dissolving in 80mL of deionized water, and performing ultrasonic dispersion for 1h to obtain a solution A;
(3) weighing 3.04g of thiourea, adding the thiourea into the solution A obtained in the step (2), and stirring for 3 hours to obtain a solution B;
(4) transferring the solution B obtained in the step (3) into a reaction kettle, carrying out hydrothermal reaction at 200 ℃ for 24h, and naturally cooling to room temperature after the reaction is finished to obtain a precipitate C;
(5) and (4) carrying out centrifugal washing on the precipitate C obtained in the step (4) by using deionized water and absolute ethyl alcohol in sequence, and then placing the precipitate C in a vacuum drying oven at 90 ℃ for drying for 12 hours to obtain the tin disulfide/carbon composite material.
Example 5
A preparation method of a tin disulfide/carbon composite negative electrode material of a lithium ion battery comprises the following steps:
(1) mixing tributyltin chloride, dimethyl tin oxide and disodium stannous citrate powder according to the molar ratio of 1:1:1, putting the mixture into a tube furnace, calcining the mixture for 1h at 800 ℃ in argon-hydrogen (volume ratio of 19:1), heating at the rate of 2 ℃/min, naturally cooling the tube furnace to room temperature, taking out a sample, and cleaning the sample with deionized water at 40 ℃ to obtain the tin-carbon composite material.
(2) Weighing 1.4875g of tin-carbon composite material, dissolving in 50mL of deionized water, and performing ultrasonic dispersion for 1h to obtain a solution A;
(3) weighing 2.28g of thiourea, adding the thiourea into the solution A obtained in the step (2), and stirring for 1h to obtain a solution B;
(4) transferring the solution B obtained in the step (3) into a reaction kettle, carrying out hydrothermal reaction at 180 ℃ for 24h, and naturally cooling to room temperature after the reaction is finished to obtain a precipitate C;
(5) and (4) carrying out centrifugal washing on the precipitate C obtained in the step (4) by using deionized water and absolute ethyl alcohol in sequence, and then placing the precipitate C in a vacuum drying oven at 80 ℃ for drying for 10 hours to obtain the tin disulfide/carbon composite material.
Example 6
A preparation method of a tin disulfide/carbon composite negative electrode material of a lithium ion battery comprises the following steps:
(1) and (2) putting tributyltin oxide into a tube furnace, calcining for 0.5h at 700 ℃ under the argon atmosphere, heating at the rate of 5 ℃/min, naturally cooling the tube furnace to room temperature, taking out a sample, and cleaning with deionized water at 70 ℃ to obtain the tin-carbon composite material.
(2) Weighing 1.4875g of tin-carbon composite material, dissolving in 70mL of deionized water, and performing ultrasonic dispersion for 0.5h to obtain a solution A;
(3) weighing 1.52g of thiourea, adding the thiourea into the solution A obtained in the step (2), and stirring for 2 hours to obtain a solution B;
(4) transferring the solution B obtained in the step (3) into a reaction kettle, carrying out hydrothermal reaction at 200 ℃ for 12h, and naturally cooling to room temperature after the reaction is finished to obtain a precipitate C;
(5) and (4) carrying out centrifugal washing on the precipitate C obtained in the step (4) by using deionized water and absolute ethyl alcohol in sequence, and then placing the precipitate C in a vacuum drying oven at 60 ℃ for drying for 14h to obtain the tin disulfide/carbon composite material.
Example 7
A preparation method of a tin disulfide/carbon composite negative electrode material of a lithium ion battery comprises the following steps:
(1) mixing dimethyltin dichloride and disodium stannous citrate according to the molar ratio of 1:2.25, putting the mixture into a tube furnace, calcining the mixture for 8 hours at 500 ℃ under the argon atmosphere at the heating rate of 2 ℃/min, taking out a sample after the temperature of the tube furnace is naturally cooled to the room temperature, and cleaning the sample with deionized water at 20 ℃ to obtain the tin-carbon composite material.
(2) Weighing 1.4875g of tin-carbon composite material, dissolving in 80mL of deionized water, and performing ultrasonic dispersion for 0.5h to obtain a solution A;
(3) weighing 0.76g of thiourea, adding the thiourea into the solution A obtained in the step (2), and stirring for 2 hours to obtain a solution B;
(4) transferring the solution B obtained in the step (3) into a reaction kettle, carrying out hydrothermal reaction at 200 ℃ for 8h, and naturally cooling to room temperature after the reaction is finished to obtain a precipitate C;
(5) and (4) carrying out centrifugal washing on the precipitate C obtained in the step (4) by using deionized water and absolute ethyl alcohol in sequence, and then placing the precipitate C in a vacuum drying oven at 70 ℃ for drying for 10 hours to obtain the tin disulfide/carbon composite material.
Example 8
A preparation method of a tin disulfide/carbon composite negative electrode material of a lithium ion battery comprises the following steps:
(1) and (2) mixing the disodium stannous citrate and the trichloromethyl tin according to the molar ratio of 1:0.45, putting the mixture into a tube furnace, calcining for 1h at 1200 ℃ under the argon atmosphere at the heating rate of 20 ℃/min, taking out a sample after the temperature of the tube furnace is naturally cooled to the room temperature, and cleaning with deionized water at 90 ℃ to obtain the tin-carbon composite material.
(2) Weighing 1.4875g of tin-carbon composite material, dissolving in 20mL of deionized water, and performing ultrasonic dispersion for 2h to obtain a solution A;
(3) weighing 2.28g of thiourea, adding the thiourea into the solution A obtained in the step (2), and stirring for 1h to obtain a solution B;
(4) transferring the solution B obtained in the step (3) into a reaction kettle, carrying out hydrothermal reaction for 8h at 160 ℃, and naturally cooling to room temperature after the reaction is finished to obtain a precipitate C;
(5) and (4) carrying out centrifugal washing on the precipitate C obtained in the step (4) by using deionized water and absolute ethyl alcohol in sequence, and then placing the precipitate C in a vacuum drying oven at 70 ℃ for drying for 10 hours to obtain the tin disulfide/carbon composite material.
Claims (10)
1. A preparation method of a tin disulfide/carbon composite material is characterized by comprising the following steps:
(1) putting the tin-containing compound into a tubular furnace, carrying out pyrolysis reaction under a protective atmosphere, preserving heat for a period of time, naturally cooling to room temperature after the reaction is finished, and cleaning the obtained sample with water to obtain the tin-carbon composite material;
(2) adding a certain amount of tin-carbon composite material into water, and performing ultrasonic dispersion to obtain a solution A;
(3) adding a certain amount of thiourea into the solution A obtained in the step (2), and stirring to obtain a solution B;
(4) transferring the solution B obtained in the step (3) to a reaction kettle, carrying out hydrothermal reaction, and naturally cooling to room temperature after the reaction is finished to obtain a precipitate C;
(5) and (4) carrying out centrifugal washing on the precipitate C obtained in the step (4) by using water and absolute ethyl alcohol in sequence, and then placing the precipitate C in a vacuum drying oven for drying to obtain the tin disulfide/carbon composite material.
2. The method for preparing a tin disulfide/carbon composite material according to claim 1, wherein the tin-containing compound in step (1) comprises one, two or more of dimethyltin oxide, dimethyltin dichloride, disodium stannous citrate, tributyltin oxide, butyltin trichloride, trichloromethyltin and tributyltin chloride; when the tin-containing compound is three, the molar ratio of any three tin-containing compounds is 1: (0-2.5): (0 to 3.0).
3. The preparation method of the tin disulfide/carbon composite material as claimed in claim 1, wherein the protective atmosphere in the step (1) comprises argon, nitrogen or a mixed gas of argon and hydrogen, and the volume ratio of argon to hydrogen in the mixed gas is (9-19): 1.
4. The preparation method of the tin disulfide/carbon composite material according to claim 1, wherein the reaction temperature of the pyrolysis reaction in the step (1) is 500-1200 ℃, the temperature rise rate is 2-20 ℃/min, and the heat preservation time is 0.5-8 h; the cleaning water is deionized water, and the temperature is 20-90 ℃.
5. The method for preparing the tin disulfide/carbon composite material as claimed in claim 1, wherein the mass concentration of the tin-carbon composite material in water in the step (2) is 0.125-0.5 mol/L; and (3) the time of ultrasonic dispersion in the step (2) is 0.5-2 h.
6. The preparation method of the tin disulfide/carbon composite material as claimed in claim 1, wherein the molar ratio of the thiourea in the step (3) to the elemental sulfur and the elemental tin in the tin-carbon composite material in the step (2) is (1-4): 1; and (4) stirring for 1-3 h in the step (3).
7. The method for preparing the tin disulfide/carbon composite material according to claim 1, wherein the temperature of the hydrothermal reaction in the step (4) is 160-200 ℃, and the reaction time is 8-24 h.
8. The method for preparing a tin disulfide/carbon composite material as claimed in claim 1, wherein the drying temperature in step (5) is 60-90 ℃.
9. Tin disulfide/carbon composite material produced by the production method according to any one of claims 1 to 8.
10. Use of the tin disulfide/carbon composite of claim 9 in the preparation of a lithium ion battery negative electrode.
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| CN114180618A (en) * | 2022-01-10 | 2022-03-15 | 扬州大学 | Palm-shaped SnS self-assembled on flexible substrate carbon paper2And method for preparing the same |
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| CN114180618A (en) * | 2022-01-10 | 2022-03-15 | 扬州大学 | Palm-shaped SnS self-assembled on flexible substrate carbon paper2And method for preparing the same |
| CN114180618B (en) * | 2022-01-10 | 2024-05-10 | 扬州大学 | Palm-shaped SnS self-assembled on flexible substrate carbon paper2And a method for preparing the same |
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