CN110649250A - Preparation method of graphene/sulfur composite material and application of graphene/sulfur composite material in lithium-sulfur battery - Google Patents
Preparation method of graphene/sulfur composite material and application of graphene/sulfur composite material in lithium-sulfur battery Download PDFInfo
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Abstract
The invention discloses a preparation method of a graphene/sulfur composite material and application of the graphene/sulfur composite material in a lithium-sulfur battery, wherein the preparation method of the graphene/sulfur composite material comprises the following steps: mixing formaldehyde and resorcinol, adding graphene, performing oil bath reaction to obtain organogel, drying, carbonizing at high temperature in an argon atmosphere to obtain a graphene modified carbon material, subliming and mixing the graphene modified carbon material with sulfur, and impregnating to obtain the graphene/sulfur composite material; the preparation method is simple, the prepared graphene/sulfur composite material can effectively inhibit polysulfide generated in the battery cycle process from being dissolved in electrolyte, and meanwhile, the graphene/carbon material can enhance electrode conductivity and obviously improve the charge-discharge cycle performance of the lithium-sulfur battery.
Description
Technical Field
The invention belongs to the technical field of new energy battery materials, and particularly relates to a preparation method of a graphene/sulfur composite material and application of the graphene/sulfur composite material in a lithium-sulfur battery.
Background
With the rapid development of human society and the increasing demand for fossil energy, people are facing the challenges of resource exhaustion and environmental problems. In the face of such difficulties, the awareness and demand for high specific energy chemical power sources has become even higher. Since the commercialization of lithium ion batteries, research and development work on power lithium ion batteries for vehicles has been tightened in all countries around the world. But the traditional lithium ion batteries such as lithium iron phosphate, lithium manganate and lithium cobaltate batteries can not meet the requirements of electric automobiles due to a series of factors of energy density, safety and price. The lithium-sulfur battery is concerned by high energy density, and the specific capacity of the lithium-sulfur battery can reach 1675mAh g-1。
The active material of the lithium-sulfur battery positive electrode material is sulfur element, has a plurality of advantages, is abundant in nature, environment-friendly, non-toxic and the like, and simultaneously faces some challenges. In the prior art, as a material of a sulfur positive electrode carrier of a lithium sulfur battery, polysulfide dissolved in an electrolyte is generated in the battery cycle process, so that the charge-discharge cycle performance of the lithium sulfur battery is influenced.
Disclosure of Invention
In order to solve the technical problems, the invention provides a preparation method of a graphene/sulfur composite material and application of the graphene/sulfur composite material in a lithium-sulfur battery. The preparation method is simple, the prepared graphene/sulfur composite material can effectively inhibit polysulfide generated in the battery circulation process from being dissolved in electrolyte, meanwhile, the graphene has high specific surface area, good chemical stability and excellent mechanical property and flexibility, and can be used as a coating material to form a protective layer on the surface of active material sulfur and also can be used as a support material of sulfur to provide a conductive network in a lithium sulfur battery, and finally, the polysulfide can be captured by functional groups on the surface of the graphene.
The technical scheme adopted by the invention is as follows:
a preparation method of a graphene/sulfur composite material, comprising the following steps:
(1) mixing formaldehyde and resorcinol, adding graphene, and carrying out oil bath reaction to obtain organogel;
(2) drying the organogel prepared in the step (1) under normal pressure;
(3) carbonizing the organogel obtained in the step (2) at high temperature in an argon atmosphere to obtain a graphene modified carbon material;
(4) and mixing the sublimed sulfur of the graphene modified carbon material, and soaking to obtain the graphene/sulfur composite material.
Further, in the step (1), the molar ratio of formaldehyde to resorcinol is 3-5: 1; the molar ratio of graphene to resorcinol is 1: 3-1.
In the step (1), the oil bath reaction conditions are as follows: under the constant temperature environment of 65-95 ℃, the stirring speed is 110-220r/min, and the reaction time is 6-20 h.
In the step (2), the drying process conditions of the organogel are as follows: drying at 100-150 deg.C under normal pressure for 16-24 h.
In the step (3), the high-temperature carbonization process conditions of the organogel are as follows: in a nitrogen atmosphere, at 3-8 ℃ for min-1The temperature rise rate is increased to 650-850 ℃, and carbonization is carried out for 6-12 h.
Further, the rate of temperature rise is preferably 5 ℃ min-1。
In the step (4), the mass ratio of the graphene modified carbon material to the sublimed sulfur is 1: 3-1; the impregnation conditions are as follows: dipping for 20-25h at the temperature of 150 ℃ and 165 ℃.
In the step (4), the mass ratio of the graphene modified carbon material to the sublimed sulfur is 1: 1; the impregnation conditions are as follows: soaking at 150 deg.C for 20 h.
The invention also provides a lithium-sulfur battery anode which is prepared by taking the graphene/sulfur composite material prepared by the preparation method as an active material.
The invention also provides a lithium-sulfur battery which is assembled by taking the positive electrode of the lithium-sulfur battery as the positive electrode.
Compared with the prior art, the technical scheme of the invention has the following advantages:
(1) according to the invention, the graphene modified carbon material with uniform particles can be prepared by using the preparation method, so that the particle size of the carbon material can be controlled within a certain range.
(2) According to the invention, the graphene modified carbon material is used as a sulfur matrix, the content of active substance sulfur can be controlled, and further the capacity of the battery is improved, meanwhile, the graphene modified carbon material is used as a carrier of the lithium-sulfur battery, the cycle performance and the rate performance of the battery can be obviously improved, and the capacity retention rate is better after 100 times of charge-discharge cycles.
(3) According to the invention, the graphene/sulfur composite material is used as a sulfur positive electrode carrier of the lithium-sulfur battery, so that polysulfide generated in the battery cycle process can be effectively inhibited from being dissolved in electrolyte, and meanwhile, the graphene/carbon material can enhance the electrode conductivity and obviously improve the charge-discharge cycle performance of the lithium-sulfur battery.
Drawings
Fig. 1 is a graph showing charge and discharge performance of lithium-sulfur batteries prepared from graphene/sulfur composites according to examples and comparative examples of the present invention;
fig. 2 shows the performance of the lithium-sulfur battery prepared from the graphene/sulfur composite material according to each example of the present invention and comparative example after 100 cycles;
fig. 3 is a graph showing rate cycle performance of lithium-sulfur batteries prepared from the graphene/sulfur composite in each of examples of the present invention and comparative examples;
in the figure, GR0-C/S, GR1-C/S, GR2-C/S, GR3-C/S corresponds to the graphene/sulfur composite in comparative example 1 (graphene doping amount of 0), example 1 (graphene to resorcinol molar ratio of 1:2), example 3 (graphene to resorcinol molar ratio of 1:1.5), and example 2 (graphene to resorcinol molar ratio of 1:1), respectively.
Detailed Description
The invention is described in detail below with reference to the following examples and the accompanying drawings.
Example 1
A preparation method of a graphene/sulfur composite material comprises the following steps:
(1) mixing formaldehyde and resorcinol according to a molar ratio of 2:1, and adding graphene, wherein the molar ratio of the graphene to the resorcinol is 1:2, reacting for 10 hours at a stirring speed of 160r/min under the condition of oil bath at a constant temperature of 85 ℃ to obtain organogel;
(2) drying the prepared organogel for 24 hours at 100 ℃ and normal pressure by using an oven to obtain organogel;
(3) next, the organogel in the step (2) is put in a nitrogen atmosphere at 5 ℃ for min-1And (3) heating up to 850 ℃ at a heating rate, and carbonizing for 8h at a high temperature to obtain the graphene modified carbon material.
(4) The method comprises the following steps of (1) mixing a graphene modified carbon material and sublimed sulfur according to a mass ratio of 3: 4, soaking for 20 hours at the temperature of 150 ℃ to obtain the graphene/sulfur composite material.
Example 2
A preparation method of a graphene/sulfur composite material comprises the following steps:
(1) mixing formaldehyde and resorcinol according to a molar ratio of 2:1, and adding graphene, wherein the molar ratio of the graphene to the resorcinol is 1:1, then reacting for 10 hours at a stirring speed of 160r/min under the condition of oil bath at a constant temperature of 85 ℃ to obtain organogel;
(2) drying the prepared organogel for 24 hours at 100 ℃ and normal pressure by using an oven to obtain organogel;
(3) next, the organogel in the step (2) is put in a nitrogen atmosphere at 5 ℃ for min-1And (3) heating up to 850 ℃ at a heating rate, and carbonizing for 8h at a high temperature to obtain the graphene modified carbon material.
(4) The method comprises the following steps of (1) mixing a graphene modified carbon material and sublimed sulfur according to a mass ratio of 3: 4, soaking for 20 hours at the temperature of 150 ℃ to obtain the graphene-sulfur composite material, and taking the graphene-sulfur composite material as the positive electrode of the lithium-sulfur battery.
Example 3
A preparation method of a graphene/sulfur composite material comprises the following steps:
(1) mixing formaldehyde and resorcinol according to a molar ratio of 2:1, and adding graphene, wherein the molar ratio of the graphene to the resorcinol is 1:1.5, then reacting for 10 hours at a stirring speed of 160r/min under the condition of oil bath at a constant temperature of 85 ℃ to obtain organogel;
(2) drying the prepared organogel for 24 hours at 100 ℃ and normal pressure by using an oven to obtain organogel;
(3) next, the organogel in the step (2) is put in a nitrogen atmosphere at 5 ℃ for min-1And (3) heating up to 850 ℃ at a heating rate, and carbonizing for 8h at a high temperature to obtain the graphene modified carbon material.
(4) The method comprises the following steps of (1) mixing a graphene modified carbon material and sublimed sulfur according to a mass ratio of 3: 4, soaking for 20 hours at the temperature of 150 ℃ to obtain the graphene-sulfur composite material, and taking the graphene-sulfur composite material as the positive electrode of the lithium-sulfur battery.
Comparative example 1
The procedure is otherwise as in example 1, except that the amount of graphene used is 0.
Example 4
Application of graphene/sulfur composite material in lithium-sulfur battery
Taking the graphene/sulfur composite materials prepared in the above examples and comparative examples as active materials, respectively, the following active materials were added: acetylene black: uniformly mixing the PVDF in a mass ratio of 7:2:1, smearing, and drying in vacuum to obtain the positive plate. A lithium sheet is taken as a negative electrode, a Celgard 2400 microporous polypropylene membrane is taken as a diaphragm, 1mol/L LiPF6/EC + DMC + EMC (1: 1:1, volume ratio) is taken as electrolyte, and the CR 2025 button lithium-sulfur battery is assembled in a glove box filled with argon.
Then, the cycle performance and the charge-discharge performance of the lithium-sulfur battery were tested at a current of 0.2C, and the results are shown in fig. 1-3, and it can be seen from fig. 1 that the first discharge capacities of the lithium-sulfur batteries prepared from the graphene/sulfur composite materials in examples 1, 2, and 3 were 1234mAh/g, 1100mAh/g, and 1411mAh/g, respectively, and all had higher charge-discharge capacities and were all better than the lithium-sulfur battery prepared from the material in comparative example 1, and the charge-discharge capacities were measured at a graphene: the molar ratio of resorcinol is 1:1.5 corresponds to the maximum first discharge capacity of the lithium-sulfur battery.
As can be seen from fig. 2, after 100 cycles, the capacity retention rates of the lithium-sulfur batteries prepared from the graphene/sulfur composite materials in the embodiments are all above 86%, and the capacity retention rate of the lithium-sulfur battery prepared from the graphene/sulfur composite material in the embodiment 3 is the best, while the capacity retention rate of the lithium-sulfur battery prepared from the material in the comparative example 1 is only 47.3%; therefore, the lithium-sulfur battery prepared from the graphene/sulfur composite material in each embodiment of the invention has good capacity retention rate after 100 charge-discharge cycles.
As can be seen from fig. 3, after the lithium-sulfur battery obtained in each example of the present invention is subjected to high-rate discharge, the lithium-sulfur battery is subjected to low-rate discharge, and the capacity is better than the previous capacity retention rate, which indicates that the battery cycle and discharge rate performance are good.
The above detailed description of a method for preparing a graphene/sulfur composite and its application in a lithium-sulfur battery with reference to examples is illustrative and not restrictive, and several examples can be cited within the scope defined, so that changes and modifications that do not depart from the general concept of the present invention are intended to be within the scope of the present invention.
Claims (10)
1. A preparation method of a graphene/sulfur composite material is characterized by comprising the following steps:
(1) mixing formaldehyde and resorcinol, adding graphene, and carrying out oil bath reaction to obtain organogel;
(2) drying the organogel prepared in the step (1) under normal pressure;
(3) carbonizing the organogel obtained in the step (2) at high temperature in an argon atmosphere to obtain a graphene modified carbon material;
(4) and mixing the sublimed sulfur of the graphene modified carbon material, and soaking to obtain the graphene/sulfur composite material.
2. The process according to claim 1, wherein in the step (1), the molar ratio of formaldehyde to resorcinol is 3-5: 1; the molar ratio of the graphene to the resorcinol is 1: 3-1.
3. The production method according to claim 1 or 2, characterized in that, in the step (1), the oil bath reaction conditions are: under the constant temperature environment of 65-95 ℃, the stirring speed is 110-220r/min, and the reaction time is 6-20 h.
4. The preparation method according to claim 1 or 2, wherein in the step (2), the drying process conditions of the organogel are as follows: drying at 100-150 deg.C under normal pressure for 16-24 h.
5. The preparation method according to claim 1 or 2, wherein in the step (3), the organogel high-temperature carbonization process conditions are as follows: in a nitrogen atmosphere, at 3-8 ℃ for min-1The temperature rise rate is increased to 650-850 ℃, and carbonization is carried out for 6-12 h.
6. The method according to claim 5, wherein the temperature increase rate is 5 ℃ min-1。
7. The production method according to claim 1, wherein in the step (4), the mass ratio of the graphene-modified carbon material to the sublimed sulfur is 1: 3-1; the impregnation conditions are as follows: dipping for 20-25h at the temperature of 150 ℃ and 165 ℃.
8. The production method according to claim 1 or 7, wherein in the step (4), the mass ratio of the graphene-modified carbon material to the sublimed sulfur is 1: 1; the impregnation conditions are as follows: soaking at 150 deg.C for 20 h.
9. A positive electrode for a lithium-sulfur battery, characterized by being prepared using the graphene/sulfur composite material prepared by the preparation method according to any one of claims 1 to 8 as an active material.
10. A lithium-sulfur battery, characterized by being assembled with the positive electrode of the lithium-sulfur battery according to claim 9 as a positive electrode.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN112421041A (en) * | 2020-11-17 | 2021-02-26 | 奇瑞商用车（安徽）有限公司 | B-Mo-C carrier and preparation method and application thereof |
| CN114784254A (en) * | 2022-05-24 | 2022-07-22 | 奇瑞商用车（安徽）有限公司 | Preparation method of nitrogen/graphene/carbon carrier composite material, and anode material, anode and lithium ion battery prepared by using nitrogen/graphene/carbon carrier composite material |
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Application publication date: 20200103 |