CN112174127A - Nitrogen-sulfur double-doped graphene/graphite composite material, preparation method and application - Google Patents
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Abstract
The invention discloses a nitrogen-sulfur double-doped graphene/graphite composite material, a preparation method and application thereof, wherein the preparation method comprises the following steps: (1) ultrasonically dispersing graphene oxide and thiourea in deionized water; (2) adding ascorbic acid into the solution until the ascorbic acid is completely dissolved; (3) heating the solution in water bath until the solution is viscous; (4) adding natural graphite into the viscous solution until the natural graphite is uniformly dispersed in the solution; (5) transferring the uniform viscous solution into a water bath kettle, and heating for self-assembly; (6) after the self-assembly reaction is finished, cooling to obtain black columnar hydrogel; (7) and (3) freezing and drying to obtain black columnar aerogel, and calcining to obtain the nitrogen-sulfur double-doped graphene/graphite composite material. According to the invention, the graphene/graphite composite material is subjected to doping modification, so that respective advantages of graphene and graphite can be brought into play together, the electrochemical performance of the lithium ion battery cathode material is improved, the operation process is simplified, and the method is suitable for large-scale industrial production.
Description
Technical Field
The invention relates to a nitrogen-sulfur double-doped graphene/graphite composite material, a preparation method and application, and belongs to the field of lithium ion batteries.
Background
Compared with the common battery, the lithium ion battery has the advantages of high energy density, rapid charge and discharge efficiency, long cycle life, better high and low temperature performance, environmental protection and the like, is widely applied and popularized in daily life and industry, and is in a vigorous development period. At present, new energy automobiles are vigorously developed in China, lithium ion batteries are used as main sources for providing power for the new energy automobiles, so that the energy density and the rate capability of the lithium ion batteries are very necessary to be improved, an important method for improving the energy density of the lithium ions is to improve the capacity of an electrode material, and because the specific capacity of a negative electrode is much higher than that of a positive electrode, the improvement of the capacity of the batteries mainly depends on the improvement of the composition of the negative electrode material.
The current commercialized negative electrode material is mainly graphite, which is used as the negative electrode of the power battery and mainly has the following problems: (1) the theoretical capacity of the graphite cathode is lower and is only 372mAh/g, and the current excellent commercial graphite cathode can reach more than 360mAh/g and is closer to the theoretical value. (2) The multiplying power performance is poor, and the battery is not suitable for large-current charging and discharging. (3) In an electrolyte containing an organic solvent, graphite undergoes a solvent co-intercalation phenomenon, and the graphitized layer structure is gradually exfoliated. Therefore, the modification treatment is carried out on the graphite, and the high-performance composite electrode material is developed, so that the method has important scientific significance and industrial value.
Graphene has been widely studied in lithium ion batteries because of its high thermal conductivity (5300W/mK), high electron mobility (1.5 × 104cm2/Vs), high mechanical strength, and the like. The graphene is used as a negative electrode material, has higher theoretical specific capacity, and has reversible capacity of about 744 mA.h/g, which is twice of that of the graphite negative electrode material. In addition, the graphene has high stability due to high heat conductivity, and lithium ions can be rapidly inserted and removed in the charging and discharging process due to large interlayer spacing of the graphene, so that the rate capability can be improved. However, due to the huge specific surface area, the graphene is low in coulombic efficiency for the first time, is not suitable for being used as an electrode independently, and can play a role in complementing advantages after being compounded with graphite, so that the graphene composite modified graphite cathode has positive significance.
Since the discovery of graphene, researchers have conducted a great deal of research on its modified preparation. Modification of hetero-atom doping is one of the important research directions. Through hetero-atom doping, on one hand, the conductivity of the graphene can be increased, and meanwhile, a defect structure caused by doping provides more lithium storage sites, so that the graphene has better electrochemical performance compared with the graphene.
Regarding a patent (publication number: CN104882608A) of Shanghai silicate research institute, Guo, et al, regarding nitrogen and sulfur co-doped graphene, thiourea, a formaldehyde solution and graphene oxide are mixed, and then are self-assembled at 60-100 ℃ for 6-24 hours, and then are subjected to heat treatment at 600-1000 ℃ for 1-6 hours to obtain the nitrogen and sulfur co-doped graphene.
The patent (publication number: CN108745402A) of Wang Fang of Bin State academy of academic is that urea and sodium thiosulfate are used as a nitrogen source and a sulfur source respectively, and a hydrothermal and subsequent high-temperature drying (150 ℃ -200 ℃) method is adopted to prepare the nitrogen-sulfur co-doped graphene.
Disclosure of Invention
Aiming at the problems in the prior art, the invention provides a nitrogen-sulfur double-doped graphene/graphite composite material, a preparation method and application thereof.
In order to achieve the purpose, the preparation method of the nitrogen-sulfur double-doped graphene/graphite composite material comprises the following steps:
(1) ultrasonically dispersing graphene oxide and thiourea in deionized water until the thiourea is completely dispersed in the aqueous solution;
(2) weighing ascorbic acid, adding the ascorbic acid into the solution obtained in the step (1), and carrying out ultrasonic treatment until the ascorbic acid is completely dissolved;
(3) heating the solution obtained in the step (2) under the condition of water bath until the solution is in a viscous state;
(4) weighing a certain amount of natural graphite, adding the natural graphite into the viscous solution obtained in the step (3), and stirring the natural graphite by strong magnetic force until the natural graphite is uniformly dispersed in the solution;
(5) transferring the uniform viscous solution obtained in the step (4) into a water bath kettle, and heating for self-assembly;
(6) after the self-assembly reaction is finished, cooling to room temperature to obtain black columnar hydrogel, soaking the black columnar hydrogel in a mixed solution of deionized water and ethanol, and then freeze-drying the black columnar hydrogel for 36-48 h;
(7) and (3) after freeze drying, obtaining black columnar aerogel, putting the black columnar aerogel into a quartz boat, and calcining for 3-5h in a tube furnace to finally obtain the nitrogen-sulfur double-doped graphene/graphite composite material.
Further, the mass ratio of the graphene oxide to the thiourea in the step (1) is 1 (1-3).
Further, the mass ratio of the ascorbic acid added in the step (2) to the graphene oxide in the step (1) is 2: 1.
Further, the temperature of water bath heating in the step (3) is 40-60 ℃, and the time is 1-2 hours.
Further, the mass ratio of the addition amount of the natural graphite in the step (4) to the graphene oxide in the step (1) is 7: 1; and (4) stirring for 1-2 hours at the rotating speed of 400-500 rpm for strong magnetic stirring in the step (4).
Further, the temperature of water bath heating in the step (5) is 80-90 ℃, and the heating time is 2-3 hours.
Further, the volume ratio of the deionized water to the alcohol in the step (6) is 5:1, and the freeze drying condition is-58 ℃ and the vacuum degree is less than or equal to 10 pa.
Further, the calcining in the step (7) is carried out under the protection of argon, the heating rate is 5 ℃/min, and the temperature is increased to 600-800 ℃.
In addition, the invention also provides a nitrogen-sulfur double-doped graphene/graphite composite material prepared by the preparation method.
Finally, the invention also provides application of the nitrogen-sulfur double-doped graphene/graphite composite material in a lithium ion battery cathode material.
Compared with the prior art, the graphene/graphite composite material is doped with the nitrogen and sulfur elements, the conductivity of the graphene is improved by doping the nitrogen elements, more active sites are added to the graphene by doping the sulfur elements, the graphene is in a fold shape, the structure is favorable for wetting the electrolyte, a channel is provided for lithium ion transmission, the rate capability of a graphite cathode is improved, and the graphene/graphite composite material is suitable for large-current charge and discharge.
Drawings
FIG. 1 is a scanning electron microscope image of the nitrogen-sulfur doped graphene/graphite composite material, wherein the ratio of rGO to thiourea is 1: 2;
fig. 2 and 3 are EDS diagrams of the nitrogen-sulfur doped graphene/graphite composite material of the present invention, and the ratio of rGO to thiourea is 1: 2.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is described in further detail below. It should be understood, however, that the description herein of specific embodiments is only intended to illustrate the invention and not to limit the scope of the invention.
Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs, and the terms used herein in the specification of the present invention are for the purpose of describing particular embodiments only and are not intended to limit the present invention.
A preparation method of a nitrogen-sulfur double-doped graphene/graphite composite material comprises the following steps:
(1) ultrasonically dispersing graphene oxide and thiourea prepared by a modified Hummers method in deionized water according to a mass ratio of 1 (1-3) until the thiourea is completely dispersed in the water solution;
(2) weighing ascorbic acid with the mass 2 times that of the graphene oxide, adding the ascorbic acid into the solution obtained in the step (1), and performing ultrasonic treatment until the ascorbic acid is completely dissolved;
(3) heating the solution obtained in the step (2) in a water bath at 40-60 ℃ for 1-2 h until the solution is viscous;
(4) weighing natural graphite with the mass 7 times that of the graphene oxide, adding the natural graphite into the viscous solution obtained in the step (3), and stirring the natural graphite with strong magnetic force for 1-2 hours at 400-500 rpm until the natural graphite is uniformly dispersed in the solution;
(5) transferring the uniform viscous solution obtained in the step (4) into a water bath kettle, heating at 80-90 ℃ for 2-3 h, and carrying out self-assembly reaction;
(6) after the self-assembly reaction is finished, cooling to room temperature to obtain black columnar hydrogel, soaking in a mixed solution of deionized water and ethanol according to a volume ratio of 5:1, and freeze-drying at-58 ℃ under a vacuum degree of less than or equal to 10pa for 36-48 h;
(7) and (3) after freeze drying, obtaining black columnar aerogel, putting the black columnar aerogel into a quartz boat, heating the quartz boat to 600-800 ℃ in a tube furnace at a heating rate of 5 ℃/min, and calcining for 3-5h to finally obtain the nitrogen-sulfur double-doped graphene/graphite composite material.
Example 1
A preparation method of a nitrogen-sulfur double-doped graphene/graphite composite material comprises the following steps:
(1) ultrasonically dispersing 0.1g of graphene oxide prepared by adopting a modified Hummers method and 0.1g of thiourea in 20ml of deionized water until the thiourea is completely dispersed in the aqueous solution;
(2) weighing 0.2g of ascorbic acid, adding the ascorbic acid into the solution obtained in the step (1), and carrying out ultrasonic treatment for 1h until the ascorbic acid is completely dissolved;
(3) heating the solution obtained in the step (2) in a water bath at 50 ℃ for 1h until the solution is in a viscous state;
(4) weighing 0.7g of natural graphite, adding the natural graphite into the viscous solution obtained in the step (3), and magnetically stirring the solution at the rotating speed of 500rpm for 1 hour until the natural graphite is uniformly dispersed in the solution;
(5) transferring the uniform viscous solution obtained in the step (4) into a water bath kettle, and heating at 90 ℃ for self-assembly for 2 hours;
(6) after the self-assembly reaction is finished, cooling to room temperature to obtain black columnar hydrogel, soaking in a solution of deionized water and ethanol (V% ═ 5:1) for 12 hours, and then freeze-drying for 36 hours;
(7) and (3) after freeze drying, obtaining black columnar aerogel, putting the black columnar aerogel into a quartz boat, and calcining for 3 hours in an argon-filled tube furnace at the temperature rising rate of 5 ℃/min to 800 ℃ to finally obtain the nitrogen-sulfur double-doped graphene/graphite composite material.
Example 2
A preparation method of a nitrogen-sulfur double-doped graphene/natural graphite composite material comprises the following steps:
(1) ultrasonically dispersing 0.1g of graphene oxide prepared by a modified Hummers method and 0.2g of thiourea in 20ml of deionized water until the thiourea is completely dispersed in the aqueous solution;
(2) weighing 0.2g of ascorbic acid, adding the ascorbic acid into the solution obtained in the step (1), and carrying out ultrasonic treatment for 1h until the ascorbic acid is completely dissolved;
(3) heating the solution obtained in the step (2) in a water bath at 50 ℃ for 1h until the solution is in a viscous state;
(4) weighing 0.7g of natural graphite, adding the natural graphite into the viscous solution obtained in the step (3), and magnetically stirring for 2 hours at the rotating speed of 400rpm until the natural graphite is uniformly dispersed in the solution;
(5) transferring the uniform viscous solution obtained in the step (4) into a water bath kettle, and heating at 85 ℃ for self-assembly for 2.5 hours;
(6) after the self-assembly reaction is finished, cooling to room temperature to obtain black columnar hydrogel, soaking in a solution of deionized water and ethanol (V% ═ 5:1) for 12 hours, and then freeze-drying at-58 ℃ and under the vacuum degree of less than or equal to 10pa for 48 hours;
(7) and (3) after freeze drying, obtaining black columnar aerogel, putting the black columnar aerogel into a quartz boat, and calcining for 4 hours in an argon-filled tube furnace at the temperature rising rate of 5 ℃/min to 700 ℃ to finally obtain the nitrogen-sulfur double-doped graphene/graphite composite material.
Example 3
A preparation method of a nitrogen-sulfur double-doped graphene/natural graphite composite material comprises the following steps:
(1) ultrasonically dispersing 0.1g of graphene oxide prepared by a modified Hummers method and 0.3g of thiourea in 20ml of deionized water until the thiourea is completely dispersed in the aqueous solution;
(2) weighing 0.2g of ascorbic acid, adding the ascorbic acid into the solution obtained in the step (1), and carrying out ultrasonic treatment for 1h until the ascorbic acid is completely dissolved;
(3) heating the solution obtained in the step (2) in a water bath at 40 ℃ for 2h until the solution is in a viscous state;
(4) weighing 0.7g of natural graphite, adding the natural graphite into the viscous solution obtained in the step (3), and magnetically stirring the solution at the rotating speed of 450rpm for 1.5 hours until the natural graphite is uniformly dispersed in the solution;
(5) transferring the uniform viscous solution obtained in the step (4) into a water bath kettle, and heating at 80 ℃ for self-assembly for 3 hours;
(6) after the self-assembly reaction is finished, cooling to room temperature to obtain black columnar hydrogel, soaking in a solution of deionized water and ethanol (V% ═ 5:1) for 12 hours, and then freeze-drying for 40 hours;
(7) and (3) after freeze drying, obtaining black columnar aerogel, putting the black columnar aerogel into a quartz boat, and calcining for 5 hours in an argon-filled tube furnace at the temperature rise rate of 5 ℃/min to 600 ℃ to finally obtain the nitrogen-sulfur double-doped graphene/graphite composite material.
The performance analysis of the nitrogen-sulfur double-doped graphene/natural graphite composite material prepared in the above examples 1 to 3 was performed: as can be seen from the scanning electron microscope in fig. 1, the active material is composed of graphene and graphite, and the graphene is distributed in a corrugated shape, which is beneficial to the hydrophilicity of the electrolyte and the transmission of lithium ions; it can be seen from the EDS spectra of fig. 2 and 3 that the material is composed of C, O, N, S four elements, illustrating that N, S two elements are effectively introduced by incorporating thiourea in the synthesis.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents or improvements made within the spirit and principle of the present invention should be included in the scope of the present invention.
Claims (10)
1. The preparation method of the nitrogen-sulfur double-doped graphene/graphite composite material is characterized by comprising the following steps of:
(1) ultrasonically dispersing graphene oxide and thiourea in deionized water until the thiourea is completely dispersed in the aqueous solution;
(2) weighing ascorbic acid, adding the ascorbic acid into the solution obtained in the step (1), and carrying out ultrasonic treatment until the ascorbic acid is completely dissolved;
(3) heating the solution obtained in the step (2) under the condition of water bath until the solution is in a viscous state;
(4) weighing a certain amount of natural graphite, adding the natural graphite into the viscous solution obtained in the step (3), and stirring the natural graphite by strong magnetic force until the natural graphite is uniformly dispersed in the solution;
(5) transferring the uniform viscous solution obtained in the step (4) into a water bath kettle, and heating for self-assembly;
(6) after the self-assembly reaction is finished, cooling to room temperature to obtain black columnar hydrogel, soaking the black columnar hydrogel in a mixed solution of deionized water and ethanol, and then freeze-drying the black columnar hydrogel for 36-48 h;
(7) and (3) after freeze drying, obtaining black columnar aerogel, putting the black columnar aerogel into a quartz boat, and calcining for 3-5h in a tube furnace to finally obtain the nitrogen-sulfur double-doped graphene/graphite composite material.
2. The preparation method of the nitrogen-sulfur double-doped graphene/graphite composite material according to claim 1, wherein the mass ratio of the graphene oxide to the thiourea in the step (1) is 1 (1-3).
3. The preparation method of the nitrogen-sulfur double-doped graphene/graphite composite material according to claim 1, wherein the mass ratio of the ascorbic acid added in the step (2) to the graphene oxide in the step (1) is 2: 1.
4. The preparation method of the nitrogen-sulfur double-doped graphene/graphite composite material according to claim 1, wherein the water bath heating in the step (3) is performed at a temperature of 40-60 ℃ for 1-2 hours.
5. The preparation method of the nitrogen-sulfur double-doped graphene/graphite composite material according to claim 1, wherein the mass ratio of the addition amount of the natural graphite in the step (4) to the graphene oxide in the step (1) is 7: 1; and (4) stirring for 1-2 hours at the rotating speed of 400-500 rpm for strong magnetic stirring in the step (4).
6. The preparation method of the nitrogen-sulfur double-doped graphene/graphite composite material according to claim 1, wherein the water bath heating temperature in the step (5) is 80-90 ℃, and the heating time is 2-3 h.
7. The preparation method of the nitrogen-sulfur double-doped graphene/graphite composite material according to claim 1, wherein the volume ratio of the deionized water to the alcohol in the step (6) is 5:1, and the freeze drying conditions are-58 ℃ and the vacuum degree is less than or equal to 10 pa.
8. The preparation method of the nitrogen-sulfur double-doped graphene/graphite composite material according to claim 1, wherein the calcination in the step (7) is performed under the protection of argon gas, the temperature rise rate is 5 ℃/min, and the temperature rises to 600-800 ℃.
9. A nitrogen-sulfur double-doped graphene/graphite composite material, which is prepared by the preparation method of any one of claims 1 to 8.
10. The use of the nitrogen-sulfur double-doped graphene/graphite composite material according to any one of claims 1 to 9 in a negative electrode material of a lithium ion battery.
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| CN115025754A (en) * | 2021-12-28 | 2022-09-09 | 淮阴师范学院 | Preparation method of patterned nitrogen and sulfur co-doped graphene aerogel |
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| CN115025754A (en) * | 2021-12-28 | 2022-09-09 | 淮阴师范学院 | Preparation method of patterned nitrogen and sulfur co-doped graphene aerogel |
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