CN110040716B - Preparation method of ultrathin carbon nanosheet negative electrode material for sodium ion battery - Google Patents
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Abstract
A preparation method of an ultrathin carbon nanosheet anode material for a sodium ion battery comprises the following steps: 1) respectively dissolving glucose and potassium hydroxide in an ethanol-water mixed solvent, fully stirring and uniformly mixing; 2) pretreating the precursor in an oven at 80-200 ℃ to obtain a precursor 3), and then carrying out one-step pyrolysis and carbonization on the precursor in a tubular atmosphere furnace at the carbonization temperature of 600 ℃ and 900 ℃ to obtain a carbonized product; 4) and (4) carrying out suction filtration and washing on the carbonized product to be neutral, and drying and grinding to obtain the ultrathin carbon nanosheet sodium ion battery cathode material. The method is simple to operate, and the prepared product is uniform in morphology distribution and small in lamella thickness (20-50 nm). The three-dimensional communicated structure and the larger specific surface area provide favorable conditions for the rapid transmission of sodium ions, can obviously improve the electrochemical performance of the material, and has the advantages of low cost and large-scale production.
Description
Technical Field
The invention belongs to the technical field of preparation of cathode materials of sodium-ion batteries, and particularly relates to a preparation method of an ultrathin carbon nanosheet cathode material for a sodium-ion battery.
Technical Field
With the heavy use of fossil fuels and the emergence of global environmental problems, it is urgent to replace traditional energy sources with renewable energy sources as main energy sources. To effectively utilize these uninterrupted sources of renewable energy and a wide range of electric or hybrid electric vehicles, advanced energy storage systems should be developed. Because of high energy density and low self-discharge rate, Lithium Ion Batteries (LIBs) have been widely used in millions of portable electronic devices and electric vehicles since 1991 (Dunn B, tamascon J m. electrical energy storage for the grid: a battery of choice [ J ] Science,2011,334(6058): 928-35.). Lithium ion battery technology has attracted researchers' attention worldwide, however, LIBs cost has risen due to limited lithium content (0.0065%) and uneven distribution of lithium resources on the earth. Sodium is abundant in resource reserves and has chemical properties similar to lithium. Therefore, Sodium Ion Batteries (SIBs) are considered to be a desirable choice for cost-effective energy storage.
However, for practical systems and further development studies, it was found that cycling stability, rate capability and capacity of SIBs still need to be enhanced. Namely, high-performance and low-cost electrode materials, particularly suitable anode materials, are urgently needed to be developed. Carbon materials are considered to be the most promising anode materials for SIBs in practical applications. Various carbon materials have been studied, including graphite, expanded graphite, amorphous carbon, and graphene. Among all carbon negative electrode candidates, hard carbon has attracted much attention due to high electrochemical activity and relatively low cost. Hard carbon contains a large amount of disordered structure, defects and voids, which contribute to a high reversible capacity. But different morphological structures have a greater impact on initial irreversible capacity loss. Wenzel et al (Wenzel S, Hara T, Janek J, et al. from-temperature sources-ion batteries: Improving the rate capability of carbon anode materials by testing the structures [ J ]. Energy & Environmental Science,2011,4(9): 3342) 3345.) have demonstrated that high loadings of carbon anode materials can be obtained by incorporating a hierarchical porous structure. Hollow Carbon Nanospheres (Tang K, Fu L, White R J, et al. Hollow Carbon Nanospheres with Superior ray Capability for Carbon-Based nanoparticles [ J ]. Advanced Energy Materials,2012,2(7): 873. 877.), Carbon nanofibers (Chen T, Liu Y, Pan L, et al. electronic nanofibers with Superior cell Capability for Carbon Materials [ J ]. Journal of Materials Chemistry A,2014,2(12): 4117. 4121.), bulk Carbon (Zhou X, Guo Y. high Carbon nanoparticles A,2014,2(12): intussum 4121.), 2015,51(89): 16045-. The carbon materials with different morphologies show excellent electrochemical performance when used as the negative electrode of the sodium-ion battery.
The layered porous structure is designed by optimizing Na+To improve the storage capacity of the carbon-based material. Thus, the rate performance of carbonaceous anode materials for SIBs can also be improved by designing mixed nanostructures comprising porous nanoplatelets.
Disclosure of Invention
The invention aims to provide a preparation method of an ultrathin carbon nanosheet negative electrode material for a sodium ion battery, which is easy to implement, low in cost and high in conductivity, and the prepared ultrathin carbon nanosheet negative electrode material can effectively improve diffusion transmission of ions and electrons and improve the performance of the battery.
In order to achieve the purpose, the invention adopts the following technical scheme:
1) respectively dissolving 1g of glucose and 0.3-1 g of potassium hydroxide in two 10-50 ml of ethanol-water mixed solvents, and uniformly stirring to respectively prepare a glucose solution and a potassium hydroxide solution;
2) mixing and stirring the glucose solution and the potassium hydroxide solution uniformly to obtain a precursor B;
3) putting the precursor B into an oven, and pretreating at 80-200 ℃ to obtain a tan product C;
4) transferring the product C into a crucible, then putting the crucible into a vacuum tube furnace, heating the product C from room temperature to 600-900 ℃ at a heating rate of 2-10 ℃/min under the protection of argon, preserving the heat for 1-3 h, then cooling the product C to 300 ℃ at a cooling rate of 10 ℃/min, and naturally cooling the product C to room temperature to obtain hard carbon nanosheets;
5) and (3) respectively filtering and washing the hard carbon nanosheets to be neutral by using deionized water and absolute ethyl alcohol, and drying to obtain the ultrathin carbon nanosheet cathode material for the sodium ion battery.
And (2) respectively grinding the glucose and the potassium hydroxide in the step 1) for 30-60 min.
The ethanol-water mixed solvent in the step 1) is water: the absolute ethyl alcohol is prepared according to the weight ratio of 1-9: 1 by volume ratio.
And 2) stirring by adopting magnetic stirring for 0.5-2.0 h.
And in the step 3), the pretreatment time is 60-180 min.
The crucible in the step 4) is an aluminum oxide crucible.
The flow rate of the argon gas in the step 4) is 0.1-1.0 sccm/min.
The drying temperature in the step 5) is 80-120 ℃, and the time is 8-12 h.
The thickness of the ultrathin carbon nanosheet negative electrode material sheet layer for the sodium ion battery in the step 5) is 20-50 nm.
The beneficial effects of the invention are as follows:
1) the invention adopts a simple one-step solid-phase preparation process, does not need to add other templates and surfactants, completes the pyrolysis and carbonization reactions in one step in a vacuum tube furnace, does not need other post-treatment, and reduces the production cost;
2) the thickness of the ultrathin hard carbon nanosheet prepared by the method is 20-50 nm. A three-dimensional interconnected network structure is formed among the carbon nano sheets, and the three-dimensional porous structure enables the carbon nano sheets to have a larger specific surface area, can be fully contacted with an electrode material and provides more attachment sites for sodium ions, so that the electrode reaction efficiency is improved, and the electrode material has higher capacity. The existence of the three-dimensional porous structure is beneficial to the diffusion of electrolyte and the migration of sodium ions, the desorption of the sodium ions is promoted, and the three-dimensional porous structure has good rate performance, can reduce the ohmic internal resistance of the electrode material and has excellent conductivity, so that the carbon material prepared under the condition has good electrochemical performance.
3) The raw materials adopted by the invention are glucose and potassium hydroxide with stable chemical components, and the method has the advantages of simple process flow, low reaction temperature, short time, no need of subsequent treatment, environmental friendliness and easiness in industrial production.
Drawings
Fig. 1 is an XRD pattern of the ultrathin carbon nanosheet anode material for the sodium ion battery prepared in example 1 of the present invention;
fig. 2 is an SEM image of the ultrathin carbon nanosheet anode material for the sodium ion battery prepared in example 2 of the present invention;
fig. 3 is an SEM image of the ultrathin carbon nanosheet anode material for the sodium ion battery prepared in example 3 of the present invention;
fig. 4 is a Raman chart of the ultrathin carbon nanosheet anode material for the sodium ion battery prepared in example 1 of the present invention;
fig. 5 is a TEM image of the ultrathin carbon nanosheet anode material for the sodium ion battery prepared in example 1 of the present invention.
Detailed Description
The present invention will be described in further detail with reference to the drawings and examples, but the present invention is not limited to the examples.
Example 1:
1) mixing water: the absolute ethyl alcohol is prepared according to the following steps of 1: 1 to obtain an ethanol-water mixed solvent, then respectively grinding 1g of glucose and 0.3g of potassium hydroxide for 30min, respectively dissolving the ground glucose and potassium hydroxide in two 10ml ethanol-water mixed solvents, and uniformly stirring to prepare a glucose solution and a potassium hydroxide solution;
2) mixing the glucose solution and the potassium hydroxide solution, and magnetically stirring for 0.5h to obtain a precursor B;
3) putting the precursor B into an oven, and pretreating for 180min at 80 ℃ to obtain a tan product C;
4) transferring the product C into an aluminum oxide crucible, then putting the aluminum oxide crucible into a vacuum tube furnace, heating the product C from room temperature to 600 ℃ at the heating rate of 2 ℃/min at the argon flow rate of 0.1sccm/min, preserving the heat for 3h, then cooling the product C to 300 ℃ at the cooling rate of 10 ℃/min, and naturally cooling the product C to room temperature to obtain hard carbon nano sheets;
5) and (3) respectively filtering and washing the hard carbon nanosheets to be neutral by using deionized water and absolute ethyl alcohol, and drying at 80 ℃ for 12 hours to obtain the ultrathin carbon nanosheet cathode material for the sodium ion battery, wherein the thickness of the lamella is 20-50 nm.
From fig. 1, it can be seen that the X-ray diffraction (XRD) pattern of the prepared ultrathin carbon nanosheet anode material shows two weak broad diffraction peaks (002) and (100) at 23 ° and 44 °, respectively, indicating the amorphous nature thereof.
As can be seen from FIG. 4, two independent characteristic peaks of a D band and a G band exist in a Raman spectrum of the prepared ultrathin carbon nanosheet cathode material and are respectively located at-1346 cm-1 and-1591 cm-1. The D peak corresponds to sp3 hybridized carbon with an unordered state and the G peak corresponds to sp2 hybridized carbon with a graphitic structure. The integrated intensity ratio of the G peak to the D peak (IG/ID) can be used to assess the degree of graphitization, with higher IG/ID values indicating more graphitic structure and high graphitization indicating high electrical conductivity. Raman fitting results indicate that the prepared sample has a higher degree of graphitization, which is beneficial for charge transfer during electrochemical reactions.
Fig. 5 shows a Transmission Electron Microscope (TEM) image of the prepared ultrathin carbon nanosheet cathode material, which proves that the prepared carbon nanosheet has a small thickness, and is beneficial to electron transmission and the reduction of the Na + diffusion path.
Example 2:
1) mixing water: the absolute ethyl alcohol is prepared according to the following steps of 3: 1 to obtain an ethanol-water mixed solvent, then respectively grinding 1g of glucose and 0.5g of potassium hydroxide for 50min, respectively dissolving the ground glucose and potassium hydroxide in two 20ml ethanol-water mixed solvents, and uniformly stirring to prepare a glucose solution and a potassium hydroxide solution;
2) mixing the glucose solution and the potassium hydroxide solution, and magnetically stirring for 1h to obtain a precursor B;
3) putting the precursor B into an oven, and pretreating for 120min at 120 ℃ to obtain a tan product C;
4) transferring the product C into an aluminum oxide crucible, then putting the aluminum oxide crucible into a vacuum tube furnace, heating the product C from room temperature to 700 ℃ at the heating rate of 5 ℃/min under the argon flow rate of 0.3sccm/min, preserving the heat for 2h, then cooling the product C to 300 ℃ at the cooling rate of 10 ℃/min, and naturally cooling the product C to room temperature to obtain hard carbon nano sheets;
5) and (3) respectively filtering and washing the hard carbon nanosheets to be neutral by using deionized water and absolute ethyl alcohol, and drying at 100 ℃ for 10 hours to obtain the ultrathin carbon nanosheet cathode material for the sodium ion battery, wherein the thickness of the lamella is 20-50 nm.
As can be seen from FIG. 2, in the SEM image of the prepared ultrathin carbon nanosheet cathode material, the thickness of the interconnected carbon nanosheets is 20-50nm, the ultrathin lamella is beneficial to the transmission of electrons, and meanwhile, the Na + diffusion path can be reduced.
Example 3:
1) mixing water: the absolute ethyl alcohol is prepared according to the following steps of 5: 1 to obtain an ethanol-water mixed solvent, then respectively grinding 1g of glucose and 0.7g of potassium hydroxide for 60min, respectively dissolving the ground glucose and potassium hydroxide in two 25ml ethanol-water mixed solvents, and uniformly stirring to prepare a glucose solution and a potassium hydroxide solution;
2) mixing the glucose solution and the potassium hydroxide solution, and magnetically stirring for 1.5h to obtain a precursor B;
3) putting the precursor B into an oven, and pretreating for 120min at 160 ℃ to obtain a tan product C;
4) transferring the product C into an aluminum oxide crucible, then putting the aluminum oxide crucible into a vacuum tube furnace, heating the product C from room temperature to 800 ℃ at the heating rate of 7 ℃/min under the argon flow rate of 0.5sccm/min, preserving the heat for 1h, then cooling the product C to 300 ℃ at the cooling rate of 10 ℃/min, and naturally cooling the product C to room temperature to obtain hard carbon nano sheets;
5) and (3) respectively filtering and washing the hard carbon nanosheets to be neutral by using deionized water and absolute ethyl alcohol, and drying at 120 ℃ for 8 hours to obtain the ultrathin carbon nanosheet cathode material for the sodium ion battery, wherein the thickness of the lamella is 20-50 nm.
As can be seen from fig. 3, in the SEM image of the prepared ultrathin carbon nanosheet negative electrode material, the carbon nanosheets are three-dimensionally interconnected to form a multilevel pore, which increases the specific surface area thereof and facilitates the diffusion and transmission of the electrolyte.
Example 4:
1) mixing water: anhydrous ethanol was prepared as 9: 1 to obtain an ethanol-water mixed solvent, then respectively grinding 1g of glucose and 1g of potassium hydroxide for 40min, respectively dissolving the ground glucose and 1g of potassium hydroxide into two 30ml ethanol-water mixed solvents, and uniformly stirring to prepare a glucose solution and a potassium hydroxide solution;
2) mixing the glucose solution and the potassium hydroxide solution, and magnetically stirring for 2 hours to obtain a precursor B;
3) putting the precursor B into an oven, and pretreating for 60min at 200 ℃ to obtain a tan product C;
4) transferring the product C into an aluminum oxide crucible, then putting the aluminum oxide crucible into a vacuum tube furnace, heating the product C from room temperature to 900 ℃ at the heating rate of 10 ℃/min at the argon flow rate of 0.8sccm/min, preserving the heat for 1h, then cooling the product C to 300 ℃ at the cooling rate of 10 ℃/min, and naturally cooling the product C to room temperature to obtain hard carbon nano sheets;
5) and (3) respectively filtering and washing the hard carbon nanosheets to be neutral by using deionized water and absolute ethyl alcohol, and drying at 90 ℃ for 11 hours to obtain the ultrathin carbon nanosheet cathode material for the sodium ion battery, wherein the thickness of the lamella is 20-50 nm.
Example 5:
1) mixing water: the absolute ethyl alcohol is prepared according to the weight ratio of 8: 1 to obtain an ethanol-water mixed solvent, then respectively grinding 1g of glucose and 0.5g of potassium hydroxide for 50min, respectively dissolving the ground glucose and potassium hydroxide in two 40ml ethanol-water mixed solvents, and uniformly stirring to prepare a glucose solution and a potassium hydroxide solution;
2) mixing the glucose solution and the potassium hydroxide solution, and magnetically stirring for 2 hours to obtain a precursor B;
3) putting the precursor B into an oven, and pretreating for 120min at 120 ℃ to obtain a tan product C;
4) transferring the product C into an aluminum oxide crucible, then putting the aluminum oxide crucible into a vacuum tube furnace, heating the product C from room temperature to 800 ℃ at the heating rate of 5 ℃/min at the argon flow rate of 1sccm/min, preserving the heat for 2h, then cooling the product C to 300 ℃ at the cooling rate of 10 ℃/min, and naturally cooling the product C to room temperature to obtain hard carbon nano-sheets;
5) and (3) respectively filtering and washing the hard carbon nanosheets to be neutral by using deionized water and absolute ethyl alcohol, and drying at 110 ℃ for 9 hours to obtain the ultrathin carbon nanosheet cathode material for the sodium ion battery, wherein the thickness of the lamella is 20-50 nm.
Example 6:
1) mixing water: the absolute ethyl alcohol is prepared according to the following steps of 6: 1 to obtain an ethanol-water mixed solvent, then respectively grinding 1g of glucose and 0.7g of potassium hydroxide for 40min, respectively dissolving the ground glucose and potassium hydroxide in two 50ml ethanol-water mixed solvents, and uniformly stirring to prepare a glucose solution and a potassium hydroxide solution;
2) mixing the glucose solution and the potassium hydroxide solution, and magnetically stirring for 1h to obtain a precursor B;
3) putting the precursor B into an oven, and pretreating for 60min at 160 ℃ to obtain a tan product C;
4) transferring the product C into an aluminum oxide crucible, then putting the aluminum oxide crucible into a vacuum tube furnace, heating the product C from room temperature to 700 ℃ at the heating rate of 2 ℃/min at the argon flow rate of 1sccm/min, preserving the heat for 2.5h, then cooling the product C to 300 ℃ at the cooling rate of 10 ℃/min, and naturally cooling the product C to room temperature to obtain hard carbon nano sheets;
5) and (3) respectively filtering and washing the hard carbon nanosheets to be neutral by using deionized water and absolute ethyl alcohol, and drying at 100 ℃ for 10 hours to obtain the ultrathin carbon nanosheet cathode material for the sodium ion battery, wherein the thickness of the lamella is 20-50 nm.
Claims (9)
1. A preparation method of an ultrathin carbon nanosheet anode material for a sodium ion battery is characterized by comprising the following steps:
1) respectively dissolving 1g of glucose and 0.3-1 g of potassium hydroxide in two 10-50 ml of ethanol-water mixed solvents, and uniformly stirring to respectively prepare a glucose solution and a potassium hydroxide solution;
2) mixing and stirring the glucose solution and the potassium hydroxide solution uniformly to obtain a precursor B;
3) putting the precursor B into an oven, and pretreating at 80-200 ℃ to obtain a tan product C;
4) transferring the product C into a crucible, then putting the crucible into a vacuum tube furnace, heating the product C from room temperature to 600-900 ℃ at a heating rate of 2-10 ℃/min under the protection of argon, preserving the heat for 1-3 h, then cooling the product C to 300 ℃ at a cooling rate of 10 ℃/min, and naturally cooling the product C to room temperature to obtain hard carbon nanosheets;
5) and (3) respectively filtering and washing the hard carbon nanosheets to be neutral by using deionized water and absolute ethyl alcohol, and drying to obtain the ultrathin carbon nanosheet cathode material for the sodium ion battery.
2. The method for preparing the ultrathin carbon nanosheet anode material for the sodium-ion battery as recited in claim 1, wherein the glucose and the potassium hydroxide of step 1) are separately ground for 30-60 min.
3. The method for preparing the ultrathin carbon nanosheet anode material for the sodium-ion battery as recited in claim 1, wherein the ethanol-water mixed solvent of step 1) is water: the absolute ethyl alcohol is prepared according to the weight ratio of 1-9: 1 by volume ratio.
4. The preparation method of the ultrathin carbon nanosheet anode material for the sodium-ion battery as recited in claim 1, wherein the stirring in step 2) is performed by magnetic stirring for 0.5-2.0 h.
5. The preparation method of the ultrathin carbon nanosheet anode material for the sodium-ion battery as recited in claim 1, wherein the pretreatment time in step 3) is 60-180 min.
6. The method for preparing the ultrathin carbon nanosheet anode material for the sodium ion battery as recited in claim 1, wherein the crucible of step 4) is an alumina crucible.
7. The preparation method of the ultrathin carbon nanosheet anode material for the sodium ion battery as recited in claim 1, wherein the argon gas flow rate in step 4) is 0.1-1.0 sccm/min.
8. The preparation method of the ultrathin carbon nanosheet anode material for the sodium-ion battery as recited in claim 1, wherein the drying temperature in step 5) is 80-120 ℃ and the time is 8-12 h.
9. The preparation method of the ultrathin carbon nanosheet anode material for the sodium-ion battery as recited in claim 1, wherein the ultrathin carbon nanosheet anode material for the sodium-ion battery in step 5) has a lamella thickness of 20-50 nm.
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