CN110790262A - Preparation method for preparing nitrogen-sulfur double-doped graphene negative electrode material by low-temperature molten salt method - Google Patents
Preparation method for preparing nitrogen-sulfur double-doped graphene negative electrode material by low-temperature molten salt method Download PDFInfo
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Abstract
The invention relates to a preparation method of a nitrogen-sulfur double-doped graphene negative electrode material by a low-temperature molten salt method, which comprises the following steps: and uniformly dispersing graphene oxide in deionized water, dissolving potassium thiocyanate in the deionized water, uniformly mixing the dispersion liquid and a salt solution, and drying to obtain the compound. And then placing the compound in a tubular furnace filled with inert gas for full reaction, washing a reaction product with a large amount of deionized water after the reaction is finished, and drying to obtain the nitrogen-sulfur double-doped graphene cathode material. Compared with the prior art, the method adopts cheap and easily-obtained industrial products as raw materials, avoids high-temperature calcination, and has the characteristics of simple synthesis process, strong controllability, low cost, wide raw material range, batch preparation and the like. The prepared nitrogen-sulfur double-doped graphene serving as the lithium ion battery cathode material has the advantages of high capacity, good cycle stability and the like.
Description
Technical Field
The invention belongs to the technical field of nano material preparation, and relates to a preparation method for preparing a nitrogen-sulfur double-doped graphene negative electrode material by a low-temperature molten salt method.
Background
The lithium ion battery has the advantages of high energy density, long cycle life, environmental friendliness and the like, and is a main energy supply source of the portable electronic equipment at present. With the continuous expansion of the scales of electric vehicles and integrated storage power grids, higher requirements are put forward on the energy storage efficiency of lithium ion batteries. At present, the commercial lithium ion battery mainly adopts graphite negative electrode materials, including natural graphite, artificial graphite and the like, and the theoretical specific capacity of the lithium ion battery is 372 mAh/g.
The graphite carbon material is a good lithium ion battery cathode material due to the characteristics of low price, wide natural raw material existence, stable electrochemical performance, convenience for various functional treatments, suitability for various lithium batteries and the like. However, the graphite-based negative electrode material also has problems of poor rate performance, small reversible discharge capacity, insufficient specific capacity, and the like. Around these problems, researchers have conceived of appropriate post-treatments of the graphite surface to improve its overall chemical properties.
At present, the post-treatment mainly focuses on the following aspects: firstly, carrying out surface coating on a graphite cathode material, wherein the surface coating comprises organic coating and electrodeless coating, and preparing a core-shell structure composite material, so that the first irreversible capacity is reduced, and the electrochemical performance is improved; secondly, carrying out heteroatom doping on the graphite cathode material, wherein the doped elements can promote the electrochemical performance of the graphite material and improve the conductivity of the graphite material; thirdly, the graphite carbon material is subjected to proper oxidation reduction treatment to eliminate the defect structure on the surface of the graphite carbon material, so that the electrochemical performance of the graphite carbon material is improved.
Nitrogen is the most abundant element in nature, and in the periodic table of elements, nitrogen-doped carbon materials are easily formed due to the adjacency to carbon elements. Similarly, sulfur element, one of the most important elements in modern chemical industry and modern chemical industry, is widely distributed in nature and can be widely used for surface modification of carbon materials. The in-situ doping method and the post-treatment method are the most common methods for preparing the nitrogen-sulfur double-doped graphene at present. However, the in-situ doping method suffers from complicated operation, time consumption, low yield and high cost; the post-processing method is difficult to overcome the defect of graphene sheet layer aggregation. Wei Ai, Ting Yu, et al, adv. Mater.2014,26, 6186-doped 6192 mentions a method for preparing nitrogen and sulfur co-doped graphene anode material by high-temperature pyrolysis. The cathode material prepared by the method has excellent cycling stability and rate capability, but has the problems of time consumption, low yield and the like. Therefore, a doping method with simple operation, environment-friendly process and low cost is urgently needed to realize the preparation of the novel functionalized graphite cathode material.
The molten salt method is a nano material preparation method which has the advantages of controllable temperature, simple operation, environment-friendly process, low price and high efficiency. In order to achieve the aim, the nitrogen-sulfur double-doped graphene is prepared by (with) inorganic salt and graphene oxide in a low-temperature molten state, and the unique fold structure and the higher nitrogen-sulfur atom doping amount of the nitrogen-sulfur double-doped graphene enable the material to show good electrochemical lithium storage performance. In addition, the method has low cost, simple and convenient operation and large-scale production, and has great potential in the fields of preparation of functionalized graphite materials and electrochemical application.
Disclosure of Invention
Technical problem to be solved
In order to avoid the defects of the prior art, the invention provides the preparation method for preparing the nitrogen-sulfur double-doped graphene anode material by using the low-temperature molten salt method, which has the characteristics of low-temperature controllability, simplicity in operation, environment-friendly process, low price, high efficiency and the like, and is a preparation method with an industrial application prospect.
Technical scheme
A preparation method for preparing a nitrogen-sulfur double-doped graphene negative electrode material by a low-temperature molten salt method is characterized by comprising the following steps:
step 1: dispersing and dissolving graphene oxide in deionized water at room temperature to form dispersion liquid, and dissolving salt containing a sulfur source or a nitrogen source in deionized water according to a mass ratio of 1: 5-50 to obtain a salt solution;
step 2: adding a salt solution into the dispersion liquid of the graphene oxide, stirring at room temperature, uniformly mixing, and drying at 50-150 ℃ to obtain a compound;
and step 3: transferring the compound into a tubular furnace filled with inert gas, heating to 150-500 ℃ at a heating rate of 2-15 ℃/min, and keeping the temperature for 1-24 hours to obtain a product, and taking out the product after the product is cooled to room temperature along with a furnace body; the reaction is completed under a sealed condition;
and 4, step 4: and washing the obtained product with deionized water, filtering and drying to obtain the nitrogen-sulfur double-doped graphene used for the lithium ion battery cathode material.
The graphene oxide includes: the obtained graphene oxide is purchased in the market, and the obtained graphene is electrically or chemically oxidized or stripped.
The salts containing nitrogen and sulfur sources include but are not limited to: thiourea, ammonium thiocyanate, potassium thiocyanate, cysteine, methionine or thioacetamide.
Advantageous effects
The invention provides a preparation method of a nitrogen-sulfur double-doped graphene anode material by using a low-temperature molten salt method. And then placing the compound in a tubular furnace filled with inert gas for full reaction, washing a reaction product with a large amount of deionized water after the reaction is finished, and drying to obtain the nitrogen-sulfur double-doped graphene cathode material. Compared with the prior art, the method adopts cheap and easily-obtained industrial products as raw materials, avoids high-temperature calcination, and has the characteristics of simple synthesis process, strong controllability, low cost, wide raw material range, batch preparation and the like. The prepared nitrogen-sulfur double-doped graphene serving as the lithium ion battery cathode material has the advantages of high capacity, good cycle stability and the like.
Compared with the prior art, the invention has the following outstanding characteristics and excellent effects:
1. compared with the existing post-treatment method for preparing the functional graphene, the method has the advantages of simple process, greenness, safety and controllable low-temperature melting;
2. compared with the prior method of introducing heteroatom doping by chemical vapor deposition, the method has the advantages of low process cost, environmental protection;
3. compared with the existing heteroatom doping method, the preparation method of the invention is simple, is suitable for large-scale continuous industrial production, and the prepared cathode material has excellent comprehensive performance;
4. the nitrogen-sulfur double-doped graphene material prepared by the process disclosed by the invention is high in specific capacity, good in cycling stability and excellent in rate capability, and can be popularized and applied to new energy devices in a large scale.
Drawings
Fig. 1 is an SEM image of a nitrogen-sulfur double-doped graphene anode material prepared in example 1 of the present invention;
fig. 2 is an XRD diffractogram of the nitrogen-sulfur double-doped graphene negative electrode material prepared in example 1 of the present invention;
fig. 3 is an XPS diagram of a nitrogen-sulfur double-doped graphene anode material prepared in example 1 of the present invention;
fig. 4 is a graph of the performance of the button cell prepared in example 1 of the present invention after the first 70 times of charge and discharge cycles under a small current;
Detailed Description
The invention will now be further described with reference to the following examples and drawings:
example 1
The application of the low-temperature molten salt method for preparing the nitrogen-sulfur double-doped graphene is applied to a lithium ion battery cathode material, and an electrochemical performance test is performed on the lithium ion battery cathode material, wherein the method comprises the following steps:
(1) ultrasonically dispersing 0.3g of graphene oxide into deionized water at room temperature, and dissolving 8g of potassium thiocyanate into the deionized water;
(2) adding a potassium thiocyanate solution into the dispersion liquid of the graphene oxide, stirring the mixed solution at room temperature for 30min, uniformly mixing, and drying at 100 ℃ to obtain a compound of the graphene oxide and potassium thiocyanate;
(3) transferring the compound obtained in the step (2) into a tubular furnace filled with inert gas, heating to 175 ℃ at the heating rate of 5 ℃/min, keeping the temperature for 12 hours to obtain a product, and taking out the product after the product is cooled to room temperature along with a furnace body;
(4) washing, filtering and drying the reactant obtained in the step (3) by using a large amount of deionized water to obtain nitrogen-sulfur double-doped graphene, and grinding the nitrogen-sulfur double-doped graphene into powder to be used as a negative electrode material of a lithium ion battery for later use;
(5) performing basic performance tests on the nitrogen-sulfur double-doped graphene powder obtained in the step (4):
testing the surface morphology (SEM analysis), composition (XRD analysis) and elemental composition (XPS analysis) of the nitrogen-sulfur double-doped graphene powder;
(6) and (5) using the nitrogen-sulfur double-doped graphene powder obtained in the step (4) as a negative electrode, using a lithium sheet as a counter electrode, assembling the lithium ion battery, and testing the performance of the battery.
Fig. 1 is an SEM image of the nitrogen-sulfur double-doped graphene anode material prepared in example 1, and the result shows that the material is a wrinkled structure as a whole, and the overall morphology is not greatly changed;
fig. 2 is an XRD spectrum of the nitrogen-sulfur double-doped graphene negative electrode material prepared in example 1, and the result shows that the diffraction angle corresponding to the peak thereof is completely consistent with that of the carbon material, indicating that the prepared product is a pure-phase graphite-like carbon material;
fig. 3 is an XPS spectrum of the nitrogen-sulfur double-doped graphene anode material prepared in example 1, and the result shows that the material contains a certain proportion of nitrogen and sulfur, which indicates that the nitrogen-sulfur double-doped graphene is successfully prepared;
FIG. 4 is a graph of the cycle performance of the lithium ion battery prepared in example 1 at a current density of 100mA/g, after 70 cycles, the specific capacity was 1048.6 mAh/g.
Example 2
(1) Ultrasonically dispersing 0.3g of graphene oxide into deionized water at room temperature, and dissolving 8g of thiourea into the deionized water;
(2) adding a thiourea solution into the dispersion liquid of the graphene oxide, stirring the mixed solution at room temperature for 30min, uniformly mixing, and drying at 100 ℃ to obtain a compound of the graphene oxide and thiourea;
(3) transferring the compound obtained in the step (2) into a tubular furnace filled with inert gas, heating to 180 ℃ at the heating rate of 5 ℃/min, keeping the temperature for 12 hours to obtain a product, and taking out the product after the product is cooled to room temperature along with a furnace body;
(4) and (4) washing the reactant obtained in the step (3) with a large amount of deionized water, filtering and drying to obtain the nitrogen-sulfur double-doped graphene, and grinding the graphene into powder to obtain the powder serving as the lithium ion battery cathode material.
Example 3
(1) Ultrasonically dispersing 0.2g of graphene oxide into deionized water at room temperature, and dissolving 10g of potassium thiocyanate into the deionized water;
(2) adding a potassium thiocyanate solution into the dispersion liquid of the graphene oxide, stirring the mixed solution at room temperature for 30min, uniformly mixing, and drying at 120 ℃ to obtain a compound of the graphene oxide and potassium thiocyanate;
(3) transferring the compound obtained in the step (2) into a tubular furnace filled with inert gas, heating to 300 ℃ at the heating rate of 10 ℃/min, keeping the temperature for 12 hours to obtain a product, and taking out the product after the product is cooled to room temperature along with a furnace body;
and (4) washing the reactant obtained in the step (3) with a large amount of deionized water, filtering and drying to obtain the nitrogen-sulfur double-doped graphene, and grinding the graphene into powder to obtain the powder serving as the lithium ion battery cathode material.
Example 4:
(1) ultrasonically dispersing 0.2g of graphene oxide into deionized water at room temperature, and dissolving 10g of potassium thiocyanate into the deionized water;
(2) adding a potassium thiocyanate solution into the dispersion liquid of the graphene oxide, stirring the mixed solution at room temperature for 30min, uniformly mixing, and drying at 120 ℃ to obtain a compound of the graphene oxide and potassium thiocyanate;
(3) transferring the compound obtained in the step (2) into a tubular furnace filled with inert gas, heating to 500 ℃ at the heating rate of 10 ℃/min, keeping the temperature for 6 hours to obtain a product, and taking out the product after the product is cooled to room temperature along with a furnace body;
(4) and (4) washing the reactant obtained in the step (3) with a large amount of deionized water, filtering and drying to obtain the nitrogen-sulfur double-doped graphene, and grinding the graphene into powder to obtain the powder serving as the lithium ion battery cathode material.
Example 5
(1) Ultrasonically dispersing 0.2g of graphene oxide into deionized water at room temperature, and dissolving 8g of potassium thiocyanate into the deionized water;
(2) adding a potassium thiocyanate solution into the dispersion liquid of the graphene oxide, stirring the mixed solution at room temperature for 30min, uniformly mixing, and drying at 100 ℃ to obtain a compound of the graphene oxide and potassium thiocyanate;
(3) transferring the compound obtained in the step (2) into a tubular furnace filled with inert gas, heating to 175 ℃ at the heating rate of 5 ℃/min, keeping the temperature for 6 hours to obtain a product graphene sheet, and taking out the product after the product is cooled to room temperature along with a furnace body;
(4) and (4) washing the reactant obtained in the step (3) with a large amount of deionized water, filtering and drying to obtain the nitrogen-sulfur double-doped graphene, and grinding the graphene into powder to obtain the powder serving as the lithium ion battery cathode material.
Compared with the prior art, the specific implementation mode has the following advantages:
1. according to the invention, graphene oxide is mixed with sulfur sources and nitrogen sources from different sources to perform a melting reaction, no by-product is generated in the reaction process, and the utilization rate of the graphene oxide reaches 99.99%.
2. The method is a heteroatom doping method which is controllable at low temperature, simple to operate, environment-friendly in process, low in cost and high in efficiency.
Claims (3)
1. A preparation method for preparing a nitrogen-sulfur double-doped graphene negative electrode material by a low-temperature molten salt method is characterized by comprising the following steps:
step 1: dispersing and dissolving graphene oxide in deionized water at room temperature to form dispersion liquid, and dissolving salt containing a sulfur source or a nitrogen source in deionized water according to a mass ratio of 1: 5-50 to obtain a salt solution;
step 2: adding a salt solution into the dispersion liquid of the graphene oxide, stirring at room temperature, uniformly mixing, and drying at 50-150 ℃ to obtain a compound;
and step 3: transferring the compound into a tubular furnace filled with inert gas, heating to 150-500 ℃ at a heating rate of 2-15 ℃/min, and keeping the temperature for 1-24 hours to obtain a product, and taking out the product after the product is cooled to room temperature along with a furnace body; the reaction is completed under a sealed condition;
and 4, step 4: and washing the obtained product with deionized water, filtering and drying to obtain the nitrogen-sulfur double-doped graphene used for the lithium ion battery cathode material.
2. The preparation method for preparing the nitrogen-sulfur double-doped graphene anode material by the low-temperature molten salt method according to claim 1 is characterized by comprising the following steps: the graphene oxide includes: the obtained graphene oxide is purchased in the market, and the obtained graphene is electrically or chemically oxidized or stripped.
3. The preparation method for preparing the nitrogen-sulfur double-doped graphene anode material by the low-temperature molten salt method according to claim 1 is characterized by comprising the following steps: the salts containing nitrogen and sulfur sources include but are not limited to: thiourea, ammonium thiocyanate, potassium thiocyanate, cysteine, methionine or thioacetamide.
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Cited By (5)
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| CN111111705A (en) * | 2020-02-18 | 2020-05-08 | 西北工业大学 | Method for synthesizing transition metal sulfide hydrogen evolution catalyst by low-temperature molten salt |
| CN112093796A (en) * | 2020-09-24 | 2020-12-18 | 江苏江南烯元石墨烯科技有限公司 | Preparation method of sulfur-nitrogen doped graphene material |
| CN112174127A (en) * | 2020-09-29 | 2021-01-05 | 江苏福瑞士电池科技有限公司 | Nitrogen-sulfur double-doped graphene/graphite composite material, preparation method and application |
| CN112938969A (en) * | 2021-03-23 | 2021-06-11 | 复旦大学 | Method for preparing nitrogen-sulfur co-doped activated carbon by pore-forming/doping integrated activating agent and application of method |
| CN116161651A (en) * | 2023-03-14 | 2023-05-26 | 昆明理工大学 | Preparation method of doped perforated graphene based on waste battery negative electrode graphite |
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| CN112938969A (en) * | 2021-03-23 | 2021-06-11 | 复旦大学 | Method for preparing nitrogen-sulfur co-doped activated carbon by pore-forming/doping integrated activating agent and application of method |
| CN116161651A (en) * | 2023-03-14 | 2023-05-26 | 昆明理工大学 | Preparation method of doped perforated graphene based on waste battery negative electrode graphite |
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