CN113178571B - Hierarchical porous Fe3Se4@ NC @ CNTs composite material and preparation method and application thereof - Google Patents
Hierarchical porous Fe3Se4@ NC @ CNTs composite material and preparation method and application thereof Download PDFInfo
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Abstract
The invention discloses a hierarchical porous Fe3Se4The @ NC @ CNTs composite material, the preparation method thereof and the application thereof in the sodium ion battery. Lyophilizing Fe (NO)3)3，CNTs，CH4N2O, NaCl nano-particles are encapsulated into a polymer fiber network and then calcined in protective gas to obtain hierarchical porous Fe3Se4@ NC @ CNTs composite, Fe3Se4The nanoparticles are well coated in the porous carbon structure, and the CNTs are intertwined to form a 3D conductive network. The method is convenient and easy to operate, reaction conditions are controllable, the obtained 3D hierarchical porous structure is special, the specific surface area is large, full contact between electrolyte and active substances is facilitated, volume expansion of the material in the charging and discharging processes is effectively adapted, and when the material is used as a sodium ion battery cathode material, the electrochemical performance of the material is greatly improved.
Description
Technical Field
The invention relates to the technical field of negative electrode materials of sodium-ion batteries, in particular to hierarchical porous Fe3Se4The @ NC @ CNTs composite material and the preparation method and the application thereof.
Background
With the rapid development of portable electronic products and electric vehicles, energy storage devices, such as Lithium Ion Batteries (LIBs), Sodium Ion Batteries (SIBs), Zinc Ion Batteries (ZIBs), etc., are receiving more and more attention. Among them, SIBs are considered to be one of the most promising candidates due to the abundant reserves of sodium, good electrochemical properties and environmental friendliness. Commercially available graphite is not suitable for anodes of SIBs because the large ionic radius of sodium ions makes it difficult to deintercalate sodium ions on the graphite layer. Therefore, the development of next-generation anode materials for SIBs is urgently required.
In recent years, selenized iron-based materials have been developedIt is abundant, non-toxic and high in theoretical capacity and is considered as a potential anode material for SIBs. However, pure iron selenide has inherently low conductivity and large volume expansion during sodium intercalation/deintercalation, resulting in poor Na+Storage performance. Many strategies have been taken to suppress the above problems, such as carbon coating, compounding with carbon, etc. In addition, the three-dimensional (3D) conductive network and layered structure may further improve the electrochemical performance of the iron selenide due to its excellent conductivity and buffer matrix. Therefore, rational design of a unique 3D conductive network with porous structure may be to increase Na of iron selenide+Promising strategy for storage performance.
In the invention, unique Fe is successfully prepared by combining hole expanding treatment and freeze drying with a simple selenization process3Se4@ NC @ CNTs multilayer porous structure. The final product has ordered macroporous structure and layered 3D carbon nanotube conductive carbonaceous network, and Fe3Se4The nanoparticles are uniformly embedded therein while being doped with carbon and nitrogen. The unique continuous 3D conductive network with a multilayer porous structure can not only improve conductivity and facilitate the transport of ions and electrons, but also mitigate drastic volume changes.
Disclosure of Invention
The invention aims to provide a hierarchical porous Fe3Se4The @ NC @ CNTs composite material and the preparation method thereof are used for preparing the negative electrode material of the sodium-ion battery, and the better electrochemical performance is obtained.
In order to solve the technical problems, the technical scheme provided by the invention is as follows: hierarchical porous Fe3Se4The preparation method of the @ NC @ CNTs composite material comprises the following steps:
1) adding the polymer into deionized water, and uniformly stirring to obtain a viscous clear liquid A;
2) adding Fe (NO) into the viscous clear liquid A3)3、CNTs、CH4N2O, NaCl, stirring vigorously to obtain black gel solution B;
3) freeze-drying the gel liquid B to obtain a product C;
4) performing high-temperature selenization treatment on the product C and selenium powder under a protective atmosphere, and continuously ventilating until the system is cooled to room temperature to obtain a product D;
5) washing and drying the product D to finally obtain hierarchical porous Fe3Se4@ NC @ CNTs composites.
Further, the polymer in the step 1) is a high molecular weight organic matter, including polyacrylonitrile (PAN, M)wI50000), polyvinylpyrrolidone (PVP, M)w1300000), polyvinyl alcohol (PVA, M)w80000), one or more of; PVA is preferred.
Further, the liquid-solid ratio in the step 1) is 8-15, preferably 10-13, and more preferably 12.5.
Further, Fe (NO) in step 2)3)3，CNTs，CH4N2The mass ratio of O to NaCl is 50:1:50: 100-200: 1:50:100, preferably 50:1:50: 100-150: 1:50:100, and more preferably 100: 1:50: 100.
Further, the temperature of the freeze drying cold trap in the step 3) is-40 ℃ to-96 ℃, and the time is 20-30 hours, and further preferably 24 hours.
Further, the protective gas in the step 4) is an inert gas, and comprises one or more of argon, nitrogen and a hydrogen-argon mixed gas, and argon is preferred.
Further, the high-temperature selenization temperature in the step 4) is 600-1000 ℃, preferably 600-800 ℃, and further preferably 600 ℃. The heat treatment time is 2 to 6 hours, preferably 2 to 5 hours, and more preferably 4 hours.
Further, the mass ratio of the selenium powder to the product C in the step 4) is at least 2: 1.
Further, the drying time in step 5) is 3-5 hours, preferably 60 ℃.
Hierarchical porous Fe3Se4The @ NC @ CNTs composite material is prepared by adopting the preparation method.
Said hierarchical porous Fe3Se4Application of the @ NC @ CNTs composite material: used for preparing sodium ion battery cathode material。
Hierarchical porous Fe of the invention3Se4The @ NC @ CNTs composite material is a 3D conductive carbon network with a macroporous structure and layers, and Fe3Se4The nanoparticles are uniformly embedded therein, and the carbon nanotubes are doped with carbon and nitrogen.
Compared with the prior art, the invention has the advantages that:
1. the method has the advantages of simple raw materials, short process flow, environmental friendliness and less carried impurities;
2. the invention adopts a freeze-drying method for direct synthesis, the process is simple and easy to implement, and the product appearance is controllable;
3. the product synthesized by the method has a special structure and a hierarchical 3D porous structure, and Fe3Se4The nano particles are well coated in a porous carbon structure, CNTs are mutually wound to form a 3D conductive network, the specific surface area is large, and the structural stability is good;
4. the product synthesized by the method has uniform morphological distribution and large specific surface area, and is favorable for improving the electrochemical performance when being used as a negative electrode material of a sodium ion battery.
Drawings
FIG. 1 shows the porous Fe layer obtained in example 1 of the present invention3Se4The XRD pattern of @ C @ CNTs composite;
FIG. 2 shows the porous Fe layer obtained in example 1 of the present invention3Se4Scanning electron microscope picture of @ C @ CNTs composite material.
FIG. 3 shows the porous Fe layer obtained in example 1 of the present invention3Se4Graph of the cycle performance of @ C @ CNTs composite.
FIG. 4 shows the porous Fe layer obtained in example 2 of the present invention3Se4XRD patterns of @ NC @ CNTs composites;
FIG. 5 shows the porous Fe layer obtained in example 2 of the present invention3Se4Pictures of a scanning electron microscope and a transmission electron microscope of the @ NC @ CNTs composite material and element mapping results;
FIG. 6 shows the porous Fe obtained in the present invention in the same level as in example 23Se4Circulation performance diagram of @ NC @ CNTs composite materialSlicing;
FIG. 7 shows the hierarchical porous Fe obtained in example 3 of the present invention3Se4Scanning electron microscope picture of @ NC @ CNTs composite material.
Detailed Description
In order to facilitate an understanding of the invention, the invention will be described more fully and in detail below with reference to the accompanying drawings and preferred embodiments, but the scope of the invention is not limited to the specific embodiments below.
Example 1:
mixing PVA (M)w80000) was added to 100mL of deionized water (liquid-solid ratio 12.5), and stirred at room temperature until clear to obtain dope a. 0.1g of commercial CNTs, 10g of Fe (NO)3)3And 10g of NaCl nano-particles are added into the viscous liquid A, and the gel liquid B is obtained by vigorous stirring. Then transferring the obtained solution to a freeze dryer to treat for 24 hours by adopting freeze drying (the temperature of a cold trap is-96 ℃) to obtain a precursor. Then selenizing 1g of precursor and 2g of selenium powder at 600 ℃ for 4h under the protection of argon gas, finally washing the obtained sample for multiple times, and drying at 60 ℃ for 4h to obtain hierarchical porous Fe3Se4@ C @ CNTs composite. The obtained sample was analyzed by an X-ray diffraction analyzer of Japan science D/max-2500 type, and the obtained results are shown in FIG. 1. All diffraction peaks of the final product correspond to Fe3Se4And an amorphous carbon phase. No other miscellaneous peak is found, which indicates that the purity of the material is higher, and the stronger peak indicates that the material has good crystallinity. As shown in FIG. 2, when the sample is observed by using a Nova Nano SEM 230 scanning electron microscope of FEI company in USA, the composite material is formed by an ordered macroporous structure and a layered 3D conductive carbonaceous network, and the prepared hierarchical porous Fe3Se4The @ NC @ CNTs composite material is prepared by uniformly mixing 80 wt.% of active material, 10 wt.% of Super-P and 10wt wt.% of PVDF to prepare slurry, uniformly coating the slurry on an aluminum foil, and vacuum drying the slurry to assemble the button cell for electrochemical performance test. The voltage range of the cycle performance test is 0.005-1.5V, and the current density is 1000mA g-1After 200 times of circulation, the specific capacity can reach 464mA h g-1After 1000 times of circulation, the specific capacity can reach 414mA h g-1. The cycle performance results are shown in fig. 3, which shows good electrochemical performance.
Example 2:
mixing PVA (M)w80000) was added to 100mL of deionized water (liquid-solid ratio 12.5), and stirred at room temperature until clear to obtain dope a. 0.1g of commercial CNTs, 10g of Fe (NO)3)3，5g CH4N2O, 10g of NaCl nanoparticles are added into the viscous liquid A, and the mixture is stirred vigorously to obtain gel liquid B. Then transferring the obtained solution to a freeze dryer to treat for 24 hours by adopting freeze drying (the temperature of a cold trap is-96 ℃) to obtain a precursor. Then selenizing 1g of precursor and 2g of selenium powder at 600 ℃ for 4h under the protection of argon, finally washing the obtained sample for multiple times, and drying at 60 ℃ for 4h to obtain hierarchical porous Fe3Se4@ NC @ CNTs composites. The obtained sample was analyzed by an X-ray diffraction analyzer of Japan science D/max-2500 type, and the results are shown in FIG. 4. All diffraction peaks of the final product correspond to Fe3Se4And an amorphous carbon phase. No other miscellaneous peak is found, which indicates that the purity of the material is higher, and the stronger peak indicates that the material has good crystallinity. As shown in FIG. 5, when the sample was observed using NovaNano SEM 230 scanning electron microscope and transmission electron microscope (TEM, JEOL-JEM-2100F), which are FEI companies, it was found that the composite material was composed of a fiber network, and had a multi-stage structure, Fe3Se4The particles are well coated, a plurality of CNTs are mutually wound to form a three-dimensional conductive network with excellent conductive performance, and the element mapping result shows that N elements are uniformly doped to form atomic defects in the composite material. The prepared hierarchical porous Fe3Se4The @ NC @ CNTs composite material is prepared by uniformly mixing 80 wt.% of active material, 10 wt.% of Super-P and 10wt wt.% of PVDF to prepare slurry, uniformly coating the slurry on an aluminum foil, and vacuum drying the slurry to assemble the button cell for electrochemical performance test. The voltage range of the cycle performance test is 0.005-1.5V, and the current density is 1000mA g-1After 200 times of circulation, the specific capacity can reach 475mA h g-1After 1000 times of circulation, the specific capacity can still reach 465mA h g-1. The cycle performance results are shown in FIG. 6, which shows good resultsElectrochemical performance.
Example 3:
mixing PVA (M)w80000) was added to 100mL of deionized water (liquid-solid ratio 12.5), and stirred at room temperature until clear to obtain dope a. 0.1g of commercial CNTs and 5g of Fe (NO)3)3，5g CH4N2O, 10g of NaCl nanoparticles are added into the viscous liquid A, and the mixture is stirred vigorously to obtain a suspension B. Transferring the obtained solution to a freeze dryer, and treating for 24 hours by adopting freeze drying (the temperature of a cold trap is-96 ℃) to obtain a precursor. Finally selenizing 1g of precursor and 2g of selenium powder at 600 ℃ for 4h under the protection of argon gas, washing the obtained sample for multiple times, and drying at 60 ℃ for 4h to obtain hierarchical porous Fe3Se4@ NC @ CNTs composites. The sample was observed using a transmission electron microscope (TEM, JEOL-JEM-2100F) and the 3D conductive network porous carbon and many CNTs were found to intertwine, indicating that the 3D conductive carbonaceous network having a macroporous structure and delamination is shown in FIG. 7.
Example 4:
mixing PVA (M)w80000) was added to 100mL of deionized water (liquid-solid ratio 12.5), and stirred at room temperature until clear to obtain dope a. 0.1g of commercial CNTs and 15g of Fe (NO)3)3，5g CH4N2O, 10g NaCl, stirred vigorously to give suspension B. Transferring the obtained solution into a freeze dryer, and carrying out freeze drying (the temperature of a cold trap is-96 ℃) for 24 hours to obtain a precursor. Finally, selenizing 1g of precursor and 2g of selenium powder at 600 ℃ for 4h under the protection of argon gas, washing the obtained sample for multiple times, and drying at 60 ℃ for 4h to obtain three-dimensional porous Fe3Se4@ NC @ CNTs composites.
Example 5:
mixing PVP (M)w1300000) was added to 100mL of deionized water (liquid-solid ratio 9), and stirred at room temperature until clear to obtain viscous liquid a. 0.1g of commercial CNTs and 10g of Fe (NO)3)3，5g CH4N2O, 10g NaCl, was vigorously stirred to obtain suspension B. Transferring the obtained solution to a freeze dryer, and treating for 24 hours by adopting freeze drying (the temperature of a cold trap is-96 ℃) to obtain a precursor. Finally will beSelenizing 1g of precursor and 2g of selenium powder at 800 ℃ for 5h under the protection of argon gas, washing the obtained sample for multiple times, and drying at 60 ℃ for 4h to obtain three-dimensional porous Fe3Se4@ NC @ CNTs composite.
Example 6
Will PAN (M)w150000) was added to 100mL of deionized water (liquid-solid ratio 14), and the mixture was stirred at room temperature until it was clear to obtain viscous liquid a. 0.1g of commercial CNTs and 20g of Fe (NO)3)3，5g CH4N2O, 10g NaCl, was vigorously stirred to obtain suspension B. Transferring the obtained solution to a freeze dryer, and treating for 24 hours by adopting freeze drying (the temperature of a cold trap is-96 ℃) to obtain a precursor. Finally, selenizing 1g of precursor and 2g of selenium powder for 3 hours at 1000 ℃ under the protection of argon, washing the obtained sample for multiple times, and drying for 4 hours at 60 ℃ to obtain the three-dimensional porous Fe3Se4@ NC @ CNTs composites.
Claims (9)
1. Hierarchical porous Fe3Se4The preparation method of the @ NC @ CNTs composite material is characterized by comprising the following steps of: the method comprises the following steps:
1) adding the polymer into deionized water, and stirring uniformly to obtain viscous clear liquid A;
2) adding Fe (NO) into the viscous clear liquid A3)3、CNTs、CH4N2O and NaCl are stirred to obtain black gel liquid B;
3) freeze-drying the gel solution B to obtain a product C;
4) carrying out high-temperature selenization treatment on the product C and selenium powder under a protective atmosphere to obtain a product D;
5) washing and drying the product D to finally obtain hierarchical porous Fe3Se4@ NC @ CNTs composite;
the polymer in the step 1) is a high molecular weight organic matter, and comprises one or more of polyacrylonitrile, polyvinylpyrrolidone and polyvinyl alcohol.
2. The hierarchy of claim 1, multiPorous Fe3Se4The preparation method of the @ NC @ CNTs composite material is characterized by comprising the following steps of: the liquid-solid ratio in the step 1) is 8-15.
3. The hierarchical porous Fe of claim 13Se4The preparation method of the @ NC @ CNTs composite material is characterized by comprising the following steps of: fe (NO) in step 2)3)3,CNTs, CH4N2The mass ratio of O to NaCl is 50:1:50: 100-200: 1:50: 100.
4. The hierarchical porous Fe of claim 13Se4The preparation method of the @ NC @ CNTs composite material is characterized by comprising the following steps of: the temperature of the freeze drying cold trap in the step 3) is-40 ℃ to-96 ℃, and the time is 20-30 hours.
5. The hierarchical porous Fe of claim 13Se4The preparation method of the @ NC @ CNTs composite material is characterized by comprising the following steps of: the protective gas in the step 4) is inert gas, and comprises one or more of argon, nitrogen and hydrogen-argon mixed gas.
6. The hierarchical porous Fe of claim 13Se4The preparation method of the @ NC @ CNTs composite material is characterized by comprising the following steps of: the high-temperature selenizing temperature in the step 4) is 600-1000 ℃, and the heat treatment time is 2-6 h.
7. The hierarchical porous Fe of claim 13Se4The preparation method of the @ NC @ CNTs composite material is characterized by comprising the following steps of: the mass ratio of the selenium powder to the product C in the step 4) is at least 2: 1.
8. Hierarchical porous Fe3Se4The @ NC @ CNTs composite material is characterized in that: prepared by the preparation method of any one of claims 1 to 7.
9. The hierarchical porous Fe of claim 83Se4The application of the @ NC @ CNTs composite material is characterized in that: the method is used for preparing the negative electrode material of the sodium-ion battery.
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