CN111403730A - FePS for sodium ion battery3@ MXene nano composite anode material, preparation method thereof and sodium ion battery - Google Patents

FePS for sodium ion battery3@ MXene nano composite anode material, preparation method thereof and sodium ion battery Download PDF

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CN111403730A
CN111403730A CN202010068812.5A CN202010068812A CN111403730A CN 111403730 A CN111403730 A CN 111403730A CN 202010068812 A CN202010068812 A CN 202010068812A CN 111403730 A CN111403730 A CN 111403730A
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mxene
feps
ion battery
sodium ion
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CN111403730B (en
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李林林
马艳晨
彭生杰
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Nanjing University of Aeronautics and Astronautics
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Abstract

The invention relates to FePS for a sodium ion battery3A @ MXene nano composite negative electrode material, a preparation method thereof and a sodium ion battery, belonging to the technical field of sodium ion batteries. The FePS for the sodium ion battery of the invention3The preparation method of the @ MXene nano composite anode material comprises the following steps: adding Ti at 35-45 deg.C3AlC2With Ti3C2TxMixing MXene etching solution uniformly, and performing first solid-liquid separation; mixing the solid obtained by the first solid-liquid separation with water uniformly in inert atmosphereCarrying out medium ultrasonic treatment for 1-3h, and then carrying out secondary solid-liquid separation to obtain a liquid, namely MXene solution; FePS is prepared3And (3) uniformly mixing the aqueous dispersion of the nanosheet with the prepared MXene solution, and freeze-drying to obtain the nano/MXene composite material. The nano composite negative electrode material can provide more channels for the migration of sodium ions, and further improves the specific capacity and the cycle performance of the composite negative electrode material.

Description

FePS for sodium ion battery3@ MXene nano composite anode material, preparation method thereof and sodium ion battery
Technical Field
The invention relates to FePS for a sodium ion battery3A @ MXene nano composite negative electrode material, a preparation method thereof and a sodium ion battery, belonging to the technical field of sodium ion batteries.
Background
With the increasing importance of new energy industry in various countries around the world, more and more renewable and clean energy sources such as solar energy, wind energy, geothermal energy and the like are developed. The development of the clean energy can reduce the dependence on fossil energy reserves, but the clean energy is often limited by natural conditions in practical application, the energy storage device can improve the utilization efficiency of various energy sources and make up for the defect that the clean energy is limited by the natural conditions, and the battery is a common energy storage device.
The lithium ion battery has the advantages of high energy density, high working voltage, long cycle life, environmental friendliness and the like, and is a battery with excellent performance and wide application range. However, the shortage of metallic lithium resources on earth has limited the large-scale application of lithium ion batteries. The sodium ion battery, as a successor of the lithium ion battery, is not limited by resource reserves, and can replace the lithium ion battery in many fields. In the electrode reaction process of the sodium ion battery, the insertion/removal process of the sodium ion battery is slower due to larger radius and molar mass of sodium ions, so that the specific capacity and the cycle life of the sodium ion battery are difficult to exert higher levels, and the development of the sodium ion battery is severely restricted. In the sodium ion battery, the negative electrode material plays an important role in the capacity and the cycle life of the battery, so that the development of the negative electrode material with high specific capacity and long cycle life has very important significance in improving the performance of the sodium ion battery.
The two-dimensional nanomaterial has a special structure, can provide a more convenient and faster channel for the embedding and the separation of sodium, has good stability, and has important significance on the development of the two-dimensional nanomaterial with high specific capacity and long cycle life for a sodium-ion battery.
Disclosure of Invention
The invention provides a sodium ion batteryFePS for pool3The preparation method of the @ MXene nano composite anode material has the advantages of high specific capacity and long cycle life.
The invention also provides FePS for the sodium ion battery prepared by the preparation method3The @ MXene nano composite anode material has higher specific capacity and longer cycle life.
The technical scheme adopted by the invention for solving the technical problems is as follows:
FePS for sodium ion battery3The preparation method of the @ MXene nano composite anode material comprises the following steps:
1) adding Ti at 35-45 deg.C3AlC2With Ti3C2TxMixing MXene etching solution uniformly, and performing first solid-liquid separation; uniformly mixing the solid obtained by the first solid-liquid separation with water, carrying out ultrasonic treatment for 1-3h in an inert atmosphere, and then carrying out the second solid-liquid separation to obtain a liquid, namely MXene solution;
2) FePS is prepared3Uniformly mixing the aqueous dispersion of the nanosheets and the MXene solution prepared in the step 1), and freeze-drying to obtain the nano/MXene composite material.
The FePS for the sodium ion battery of the invention3The preparation method of the @ MXene nano composite anode material comprises the steps of preparing an MXene solution dispersed with MXene nanosheets by a liquid phase peeling method, and then mixing the MXene solution with FePS3Uniformly mixing the aqueous dispersion of the nano-sheets, and uniformly dispersing the MXene nano-sheets in the FePS3Forming FePS on the nano-sheet3@ MXene hybrid. The unique 2D/2D structure can promote the rapid transfer of electrons/ions and reduce the volume expansion of the electrode. Particularly, when the lithium ion battery is used as an anode of a sodium ion battery, the lithium ion battery can show good cycling stability and rate capability, and the sodium storage performance is more outstanding. In addition, FePS3The required electrochemical performance of the battery can be further improved. Due to the difference of the discharge potential, the generated mixed phases can be used as buffer substances of each other, and electrode powdering or agglomeration caused by volume expansion is inhibited. The ultrafine active material is uniformly distributed in the conductive MXene during the whole charging and discharging process, which ensures the rapid chargeAnd the specific capacity of the composite material is further improved.
Ti in step 1)3C2TxThe MXene etching solution is prepared by uniformly mixing hydrochloric acid and lithium fluoride, wherein the ratio of the lithium fluoride to HCl in the hydrochloric acid is 0.1-0.15mol of HCl per gram of lithium fluoride, preferably 0.12-0.14mol of HCl, the hydrochloric acid and the lithium fluoride are uniformly mixed by stirring for 3-8min, and the concentration of the hydrochloric acid is 8-10 mol/L.
Ti in step 1)3AlC2With Ti3C2TxThe MXene etching solution is evenly mixed and stirred for 30-40 h. Ti in step 1)3AlC2With Ti3C2TxThe mass ratio of the lithium fluoride in the MXene etching solution is 1: 1-2. Ti in step 1)3AlC2With Ti3C2TxAfter MXene etching solution is mixed uniformly, washing the product with water until the pH value of the washing solution is not lower than 6, and then carrying out solid-liquid separation. The inert atmosphere in step 1) is an argon atmosphere or a nitrogen atmosphere.
The amount of water when the solid obtained by the first solid-liquid separation in the step 1) is uniformly mixed with water is 2g of Ti3AlC2Correspondingly adding 220-280m L water, wherein the second solid-liquid separation in the step 1) is centrifugal separation, the rotating speed of the centrifugal separation is 3200-3600rpm, and the time of the centrifugal separation is 1-2 h.
FePS in step 2)3The dispersion liquid of the nano-sheets in water is 100-120mg of FePS3The nano-sheets are dispersed in 100-150m L ultrapure water and then are subjected to ultrasonic treatment for 20-30min to obtain the nano-particles.
FePS per 100m L in step 2)3The aqueous dispersion of the nano-sheets corresponds to MXene solution with the thickness of 3-6m L, and the uniform mixing in the step 2) is stirring for 20-30 h.
FePS in step 2)3The nanosheet is prepared by a method comprising the steps of:
FePS is prepared3The crystal is insulated for 5-7 days at 800 ℃ under the vacuum condition, then insulated for 1.5-2.5 hours at 550 ℃ under the inert atmosphere, and then dispersed in water, treated by ultrasonic treatment and freeze-dried. The ultrasonic treatment is carried out under ice bath conditions.
Sodium prepared by the preparation methodFePS for ion battery3And @ MXene nano composite negative electrode material.
The sodium ion battery comprises a positive electrode, a negative electrode, a diaphragm and electrolyte, wherein the negative electrode is FePS for the sodium ion battery3And @ MXene nano composite negative electrode material.
The invention has the beneficial effects that:
the FePS for the sodium ion battery of the invention3The @ MXene nano composite anode material has a porous layered structure, can provide more channels for the migration of sodium ions, and further improves the specific capacity and the cycle performance of the composite anode material. The FePS for the sodium ion battery of the invention3The charging and discharging specific capacity of the sodium ion battery prepared from the @ MXene nano composite negative electrode material under the current density of 0.1A/g can reach about 800 mAh/g.
Drawings
FIG. 1 shows FePS used in example 13SEM scan image of material;
FIG. 2 shows FePS for sodium ion battery prepared in example 13Scanning SEM image of @ MXene nano composite negative electrode material;
FIG. 3 shows FePS for sodium ion battery prepared in example 23A TEM image of the @ MXene nanocomposite negative electrode material;
FIG. 4 shows FePS for sodium ion battery prepared in example 13The charge-discharge curve of the sodium ion battery is prepared from the @ MXene nano composite negative electrode material;
FIG. 5 shows FePS used in example 13Materials, FePS for sodium ion Battery produced in example 13@ MXene nanocomposite negative electrode material and FePS for sodium ion battery prepared in example 23The charge-discharge cycle curve of the sodium ion battery prepared from the @ MXene nano composite anode material;
FIG. 6 shows FePS used in example 13Materials, FePS for sodium ion Battery produced in example 13@ MXene nanocomposite negative electrode material and FePS for sodium ion battery prepared in example 23The charge and discharge performance curve of the sodium ion battery prepared from the @ MXene nano composite negative electrode material under different multiplying powers is shown.
Detailed Description
In order to make the technical problems, technical solutions and advantageous effects solved by the present invention easier to understand, the present invention will be described in detail with reference to specific embodiments.
FePS in the following examples3The nanosheet is prepared by a method comprising the steps of:
mixing Fe powder, P powder and S powder according to the proportion of Fe, P and S being 1:1:3, packaging in an ampoule bottle, heating at 750 ℃ for 6d under the vacuum condition, and carrying out low-temperature solid-phase reaction to obtain three elementary substances which react to generate FePS3And (3) crystallizing, and then heating the obtained sample to 500 ℃ in an argon atmosphere, keeping the temperature for 2 hours, and removing residual sulfur and red phosphorus in the sample to obtain blocky crystals.
Dispersing 100mg of blocky crystals in 100m L deionized water, carrying out ultrasonic treatment for 8h under the ice bath condition, and then carrying out freeze drying to obtain FePS3Nanosheets.
Example 1
FePS for sodium ion battery of this example3The preparation method of the @ MXene nano composite anode material comprises the following steps:
1) adding 2g of lithium fluoride into 9.0 mol/L hydrochloric acid of 30m L, and stirring for 5min to obtain Ti3C2TxMXene etching solution.
2) At 40 ℃, 2g of Ti3AlC2Powder addition of Ti3C2TxStirring the MXene etching solution for 36 hours, washing the mixed system centrifugally separated solid after stirring for 36 hours by using water until the pH value of the washing solution is not lower than 6, then carrying out centrifugal separation, dispersing the centrifugally separated solid in 250m L deionized water, carrying out ultrasonic treatment for 2 hours under the argon atmosphere, then centrifuging at the rotating speed of 3500rpm for 1 hour, collecting the separated liquid, and freezing and storing to obtain the MXene solution.
3) 100mg of FePS3Dispersing the nano-sheets in 100m L ultrapure water, carrying out ultrasonic treatment for 30min to obtain a dispersion liquid, adding a 3m L MXene solution into the dispersion liquid, stirring for 24h, and carrying out freeze drying to obtain FePS3@ MXene sample, noted FePS3@MXene-1。
Example 2
FePS for sodium ion battery of this example3The preparation method of the @ MXene nano composite anode material comprises the following steps:
1) adding 2g of lithium fluoride into 9.0 mol/L hydrochloric acid of 30m L, and stirring for 5min to obtain Ti3C2TxMXene etching solution.
2) At 40 ℃, 2g of Ti3AlC2Powder addition of Ti3C2TxStirring the MXene etching solution for 36 hours, washing the mixed system centrifugally separated solid after stirring for 36 hours by using water until the pH value of the washing solution is not lower than 6, then carrying out centrifugal separation, dispersing the centrifugally separated solid in 250m L deionized water, carrying out ultrasonic treatment for 2 hours under the argon atmosphere, then centrifuging at 3500rpm for 1 hour, collecting the separated liquid, and freezing and storing to obtain the MXene solution.
3) 100mg of FePS3Dispersing the nano-sheets in 100m L ultrapure water, carrying out ultrasonic treatment for 30min to obtain a dispersion liquid, then adding 6m L MXene solution into the dispersion liquid, stirring for 24h, and then carrying out freeze drying to obtain FePS3@ MXene sample, noted FePS3@MXene-2。
Example 3
FePS for sodium ion battery of this example3The preparation method of the @ MXene nano composite anode material comprises the following steps:
1) adding 2g of lithium fluoride into 35m L hydrochloric acid with the concentration of 8.0 mol/L, and stirring for 8min to obtain Ti3C2TxMXene etching solution.
2) At 35 ℃, 2g of Ti3AlC2Powder addition of Ti3C2TxStirring the MXene etching solution for 32 hours, washing the centrifugally separated solid of the mixed system stirred for 36 hours by using water until the pH value of the washing solution is not lower than 6, then carrying out centrifugal separation, dispersing the centrifugally separated solid in 260m L deionized water, carrying out ultrasonic treatment for 1.5 hours under the argon atmosphere, then centrifuging the solution at the rotating speed of 3200rpm for 2 hours, collecting the separated liquid, and freezing and storing the separated liquid to obtain the MXene solution.
3) 110mg of FePS3Nanoplate dispersed in 120m L ultrapure waterPerforming ultrasonic treatment for 25min to obtain dispersion, adding 5m L MXene solution into the dispersion, stirring for 22h, and freeze drying to obtain FePS3@ MXene sample, noted FePS3@MXene-3。
Example 4
FePS for sodium ion battery of this example3The preparation method of the @ MXene nano composite anode material comprises the following steps:
1) adding 2.5g of lithium fluoride into 30m L hydrochloric acid of 10.0 mol/L, and stirring for 6min to obtain Ti3C2TxMXene etching solution.
2) At 45 ℃, 2g of Ti3AlC2Powder addition of Ti3C2TxStirring the MXene etching solution for 32 hours, washing the centrifugally separated solid of the mixed system stirred for 36 hours by using water until the pH value of the washing solution is not lower than 6, then carrying out centrifugal separation, dispersing the centrifugally separated solid in 220m L deionized water, carrying out ultrasonic treatment for 1 hour under the argon atmosphere, then centrifuging at the rotating speed of 3300rpm for 1.5 hours, collecting the separated liquid, and freezing and storing to obtain the MXene solution.
3) 100mg of FePS3Dispersing the nanosheets in 120m L ultrapure water, performing ultrasonic treatment for 20min to obtain a dispersion liquid, adding 5m L MXene solution into the dispersion liquid, stirring for 26h, and performing freeze drying to obtain FePS3@ MXene sample, noted FePS3@MXene-4。
Example 5
FePS for sodium ion battery of this example3The preparation method of the @ MXene nano composite anode material comprises the following steps:
1) adding 2g of lithium fluoride into 9.0 mol/L hydrochloric acid of 30m L, and stirring for 3min to obtain Ti3C2TxMXene etching solution.
2) At 43 ℃, 2g of Ti3AlC2Powder addition of Ti3C2TxStirring MXene etching solution for 32h, washing the mixed system centrifugally separated solid after stirring for 36h with water until the pH of the washing solution is not lower than 6, centrifugally separating, dispersing the centrifugally separated solid in 280m L to removeUltrasonically treating the seed water for 3 hours in the argon atmosphere, then centrifuging the seed water for 1.2 hours at the rotating speed of 3600rpm, collecting the separated liquid, and freezing and storing the separated liquid to obtain the MXene solution.
3) 120mg of FePS3Dispersing the nano-sheets in 150m L ultrapure water, carrying out ultrasonic treatment for 30min to obtain a dispersion liquid, then adding 5m L MXene solution into the dispersion liquid, stirring for 30h, and then carrying out freeze drying to obtain FePS3@ MXene sample, noted FePS3@MXene-5。
Example 6
The sodium ion battery of this embodiment includes a positive electrode, a negative electrode, an electrolyte, and a separator, where the negative electrode includes a negative electrode current collector and a negative electrode material layer disposed on the surface of the negative electrode current collector, the negative electrode material layer includes a negative electrode active material, a conductive agent, and a binder, and the negative electrode active material is the FePS for the sodium ion battery prepared in the foregoing embodiments 1 to 53The @ MXene nano composite negative electrode material is characterized in that a conductive agent is acetylene black, a positive electrode is a sodium sheet, a diaphragm is a Celgard2325 membrane, and an electrolyte is a sodium perchlorate electrolyte. The preparation method of the sodium-ion battery comprises the following steps: firstly adopting the FePS for the sodium ion battery3The material is characterized in that a @ MXene nano composite negative electrode material is used as an active material, acetylene black is used as a conductive agent, sodium carboxymethylcellulose is used as a binder, and the mass ratio of the active material to the acetylene black to the sodium carboxymethylcellulose is 80: 15: 5; mixing an active material, acetylene black, sodium carboxymethylcellulose and a solvent, carrying out ultrasonic treatment to obtain a negative electrode slurry, coating the negative electrode slurry on a copper foil, carrying out vacuum drying, and then carrying out tabletting on a tabletting machine; and then, preparing the button sodium-ion battery by using a sodium sheet as a counter electrode, using sodium perchlorate electrolyte as electrolyte and using Celgard2325 as a diaphragm.
Test examples
(1) Topography testing
Taking FePS used in example 13SEM scans of the material are shown in FIG. 1.
As can be seen from FIG. 1, FePS used in example 13The material has a more obvious layered structure, and the layered structure is more compact.
FePS for sodium ion Battery obtained in example 1 was used3Scanning the @ MXene nanocomposite negative electrode material by SEM, and the scanning result is shown in FIG. 2.
As can be seen from FIG. 2, FePS for sodium ion battery prepared in example 13In the @ MXene nano composite anode material, FePS3MXene nano-sheets are distributed on the lamellar structure, and the MXene nano-sheets and the lamellar structure form a relatively loose lamellar structure.
FePS for sodium ion Battery obtained in example 23The scanning result of the @ MXene nanocomposite negative electrode material by TEM scanning is shown in FIG. 3.
As can be seen from FIG. 3, FePS for sodium ion battery prepared in example 23FePS in @ MXene nano composite anode material3With MXene, a very thin nanocomposite sheet structure can be formed with more pores.
(2) Electrochemical performance test
FePS for sodium ion Battery obtained in example 1 was used3The @ MXene nanocomposite negative electrode material was used to prepare a sodium ion battery according to the method in example 5. Then, charge and discharge were performed at room temperature at a rate of 0.1C, and the charge and discharge curves are shown in fig. 4.
As can be seen from FIG. 4, FePS for sodium ion battery prepared in example 13The charging and discharging voltage platform of the sodium ion battery prepared from the @ MXene nano composite negative electrode material is not obvious, but the charging and discharging capacity can reach about 800mAh/g, and the specific capacity is higher.
Taking FePS used in example 13Materials and FePS for sodium ion Battery prepared in example 13@ MXene nanocomposite negative electrode material and FePS for sodium ion battery prepared in example 23And @ MXene nano composite negative electrode material, and the sodium ion battery is prepared according to the method in the embodiment 5. Then, a charge-discharge cycle was carried out at room temperature at a current density of 0.5A/g, and a charge-discharge cycle curve was shown in FIG. 5.
As can be seen from FIG. 5, FePS for sodium ion battery prepared by the invention3The circulating performance of the @ MXene nano composite anode material is obviously higher than that of FePS3Material, and there was only a small decay after 90 cycles.
Taking FePS used in example 13Materials and FePS for sodium ion Battery prepared in example 13@ MXene nanocomposite negative electrode material and FePS for sodium ion battery prepared in example 23And @ MXene nano composite negative electrode material, and the sodium ion battery is prepared according to the method in the embodiment 5. Then, charge and discharge cycle tests were carried out at current densities of 0.1A/g, 0.2A/g, 0.5A/g, 1A/g, 2A/g, and 5A/g, and the discharge cycle curves thereof are shown in FIG. 6.
As can be seen from FIG. 6, it is shown that3Compared with the materials, the FePS for the sodium ion battery prepared by the invention3The sodium ion battery prepared from the @ MXene nano composite anode material has better rate capability.

Claims (10)

1. FePS for sodium ion battery3The preparation method of the @ MXene nano composite anode material is characterized by comprising the following steps of: the method comprises the following steps:
1) adding Ti at 35-45 deg.C3AlC2With Ti3C2TxMixing MXene etching solution uniformly, and performing first solid-liquid separation; uniformly mixing the solid obtained by the first solid-liquid separation with water, carrying out ultrasonic treatment for 1-3h in an inert atmosphere, and then carrying out the second solid-liquid separation to obtain a liquid, namely MXene solution;
2) FePS is prepared3Uniformly mixing the aqueous dispersion of the nanosheets and the MXene solution prepared in the step 1), and freeze-drying to obtain the nano/MXene composite material.
2. FePS for sodium ion battery according to claim 13The preparation method of the @ MXene nano composite anode material is characterized by comprising the following steps of: ti in step 1)3C2TxThe MXene etching solution is prepared by uniformly mixing hydrochloric acid and lithium fluoride, and the proportion of the lithium fluoride to HCl in the hydrochloric acid is 0.1-0.15mol of HCl per gram of lithium fluoride.
3. FePS for sodium ion battery according to claim 23The preparation method of the @ MXene nano composite anode material is characterized by comprising the following steps of: ti in step 1)3AlC2With Ti3C2TxThe mass ratio of the lithium fluoride in the MXene etching solution is 1: 1-2.
4. FePS for sodium ion battery according to claim 13The preparation method of the @ MXene nano composite anode material is characterized by comprising the following steps of: the amount of water when the solid obtained by the first solid-liquid separation in the step 1) is uniformly mixed with water is 2g of Ti3AlC2Corresponding to the addition of 220 and 280m L of water.
5. FePS for sodium ion battery according to claim 13The preparation method of the @ MXene nano composite anode material is characterized by comprising the following steps of: FePS in step 2)3The aqueous dispersion of the nano-sheets consists of 100-120mg of FePS3The nano-sheets are dispersed in 100-150m L ultrapure water and then are subjected to ultrasonic treatment for 20-30min to obtain the nano-particles.
6. FePS for sodium ion battery according to claim 13The preparation method of the @ MXene nano composite anode material is characterized in that FePS of L m per 100m in the step 2)3The aqueous dispersion of the nanosheets corresponds to an MXene solution of 3-6m L.
7. FePS for sodium ion battery according to claim 13The preparation method of the @ MXene nano composite anode material is characterized by comprising the following steps of: the step 2) is to mix evenly and stir for 20 to 30 hours.
8. FePS for sodium ion battery according to any of claims 1 to 73The preparation method of the @ MXene nano composite anode material is characterized by comprising the following steps of: FePS in step 2)3The nanosheet is prepared by a method comprising the steps of: FePS is prepared3The crystal is insulated for 5-7 days at 800 ℃ under the vacuum condition, then insulated for 1.5-2.5 hours at 550 ℃ under the inert atmosphere, and then dispersed in water, treated by ultrasonic treatment and freeze-dried.
9. FePS for sodium ion battery prepared by the preparation method of claim 13And @ MXene nano composite negative electrode material.
10. A sodium ion battery comprises a positive electrode, a negative electrode, a diaphragm and electrolyte, and is characterized in that: the negative electrode is FePS for the sodium-ion battery as defined in claim 93And @ MXene nano composite negative electrode material.
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