CN113113577B - Co/CoSe/MoSe 2 Method for preparing composite material - Google Patents
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Abstract
The invention provides Co/CoSe/MoSe 2 A method for preparing a composite material. The specific process is as follows: cobalt acetate and ammonium molybdate are prepared into a mixed solution according to a proportion, and cobalt molybdate is formed by a coprecipitation method. Cobalt molybdate was added to a solution of dimethylformamide (abbreviated as DMF) mixed with polyacrylonitrile and polyvinylpyrrolidone. Then adding a proper amount of selenium powder, and preparing a fibrous mixture by electrostatic spinning after the solution is uniformly dispersed. Drying and then selenizing at high temperature to obtain Co/CoSe/MoSe 2 A composite material. Compared with MoSe as a negative electrode material of a sodium-ion battery 2 And Co/MoSe 2 The bimetallic selenide shows better electrochemical performance and has potential application value in the field of sodium-ion batteries.
Description
Technical Field
The invention relates to Co/CoSe/MoSe 2 The preparation method of the composite material is applied to the negative electrode of the sodium ion battery, and belongs to the field of sodium ion batteries.
Technical Field
With environmental pollution and energy depletion, the demand for clean energy and green and efficient energy storage systems is rapidly increasing. Among various energy storage devices, lithium ion batteries are the most mature and successful energy storage devices and are widely used in various fields. But the lithium resources on the earth are distributed unevenly and are very deficient, which limits the large-scale application of the lithium ion battery. Nowadays, the sodium ion battery is considered as a lithium ion battery substitute with development potential due to the fact that the sodium ion battery is similar to the lithium ion battery in physical and chemical properties, moderate in price and high in abundance. However, the radius of sodium ions is relatively large compared to that of lithium ions, resulting in a large volume change of the electrode and poor cycle stability. Therefore, finding electrode materials with excellent rate performance and cycling stability remains a major challenge for sodium ion batteries. The invention provides Co/CoSe/MoSe 2 Composite materialThe prepared material has good rate performance and cycling stability, and can be used as a cathode material of a sodium-ion battery.
Disclosure of Invention
The raw materials used by the invention are cobalt acetate, ammonium molybdate, selenium powder, deionized water, PAN, PVP and DMF. The preparation process comprises the following steps:
the method comprises the following steps: preparing a mixed solution from cobalt acetate and ammonium molybdate according to a proportion, forming cobalt molybdate by a coprecipitation method, drying, adding the cobalt molybdate into a DMF solution, then adding a proper amount of PAN, PVP and selenium powder, and uniformly stirring to obtain a precursor dispersion liquid;
step two: transferring the precursor dispersion liquid in the step one into an injector, fixing the injector on a micro-pump injector, connecting a positive electrode with a syringe needle, connecting a negative electrode with a collector, and collecting a fibrous mixture on the collector by adjusting the distance between the positive electrode and the negative electrode, the voltage of the positive electrode and the negative electrode, the sample injection speed of the micro-pump and the temperature of equipment;
step three: drying the fibrous mixture in the second step, peeling off the fibrous mixture from a collector, transferring the fibrous mixture to a tube furnace, and selenizing the fibrous mixture at high temperature in an inert atmosphere to obtain Co/CoSe/MoSe 2 A composite material.
In the first step, the molar ratio of cobalt acetate to ammonium molybdate is 1-2: 0.1-0.3, the temperature in the drying process is 40-100 ℃, and the drying time is 10-24 h.
When the electrostatic spinning mixed solution is prepared in the first step, the molar ratio of cobalt molybdate to selenium powder is 1-3: 2-10; the mass concentrations of PAN and PVP in the precursor dispersion liquid are 0.01-0.1g/mL and 0.01-0.05g/mL respectively.
And in the second step, the distance between the needle head connected with the anode and the collector connected with the cathode is 10-40 cm.
At a certain voltage, the spacing affects the strength of the electric field and the evaporation of the dope solvent. The appropriate distance facilitates solvent evaporation and thus deposition of the dried fiber bundle. Too short a distance causes insufficient evaporation of the solvent and the formation of fused fibers. The distance is too long, the electric field is weak, the spun silk is slightly influenced by the electric field and cannot be fully received by the collector.
In the second step, the voltage of the positive electrode is 10-30 kV, and the voltage of the negative electrode is 1-10 kV (the voltage is negative).
The electrostatic spinning is to spray protofilaments from an injector and collect the protofilaments by a collector by adjusting the voltage of a positive electrode and a negative electrode. Too small voltage is not beneficial to filament discharging, the diameter of the formed nano fiber is larger, too large voltage is not beneficial to collection, and filament discharging is not uniform, and beaded nano fibers are easy to generate.
And the sample injection speed of the micro pump in the second step is 0.1-4 mL/h.
And in the second step, the temperature of the electrostatic spinning equipment is maintained at 10-60 ℃.
In the third step, the drying temperature of the fibrous mixture is 60-100 ℃, and the drying time is 10-48 h.
The inert gas in the third step is one of nitrogen, argon or a mixed gas of the nitrogen and the argon.
The conditions of high-temperature selenization in the third step are as follows: raising the temperature from room temperature to 400-800 ℃ at the speed of 1-10 ℃/min, preserving the temperature for 1-4 h, and finally reducing the temperature to room temperature at the speed of 1-10 ℃/min.
The invention of the patent relates to Co/CoSe/MoSe 2 The preparation method of the composite material has the following characteristics:
(1) the raw material cost is low, and the cobalt source, the molybdenum source and the selenium source are rich.
(2) The preparation process has no pollution and less harm to the environment.
(3) Prepared Co/CoSe/MoSe 2 The composite material is in a submicron rod shape, the diameter is about 200 nm, the length is 3-4 mu m, the surface is smooth, and the composite material is uniformly compounded with a carbon material.
（4）、Co/CoSe/MoSe 2 Composite material, compared to MoSe 2 And Co/MoSe 2 The electrochemical performance is obviously improved.
Drawings
Figure 1 is a comparison of XRD of samples prepared in examples 1, 2, 3 with a standard card.
Fig. 2 is an SEM image of the sample prepared in example 1 before charge and discharge cycles.
FIG. 3 is a graph comparing the rate capability of samples prepared in examples 1, 2, and 3.
Fig. 4 is a charge and discharge curve for the first three cycles of the sample prepared in example 1.
Fig. 5 is a charge and discharge curve for the first three cycles of the sample prepared in example 2.
Fig. 6 is a charge and discharge curve for the first three cycles of the sample prepared in example 3.
DETAILED DESCRIPTION OF EMBODIMENT (S) OF INVENTION
Example 1
Adding 7 mmol of Co (CH) 3 COO) 2 ·4H 2 O、1 mmol (NH 4 ) 6 Mo 7 O 24 ·4H 2 Placing O in a beaker, adding 50 mL of deionized water, stirring for 4 h at 50 ℃, centrifuging at 4000 rpm to obtain cobalt molybdate, and placing in an oven to dry for 12 h at 60 ℃. Dispersing 2 mmol of cobalt molybdate in 4 ml of DMF solution, then adding 0.3 g of PAN, 0.1g of PVP and 6 mmol of selenium powder, and stirring uniformly to obtain the electrostatic spinning precursor dispersion liquid. The dispersion was transferred to a syringe and the syringe was mounted on a micropump syringe, the positive pole being connected to the syringe needle and the negative pole to the collector. The distance between the positive and negative electrodes was made 17 cm, the positive electrode voltage was 16.5 kV, the negative electrode voltage was-2.5 kV, the sample injection speed of the micro pump was 1mL/h, the equipment temperature was 30 ℃, and then the fibrous mixture was collected on a collector. Peeling the fibrous mixture from the collector, drying at 80 deg.C for 24 hr in an oven, transferring to a tube furnace, heating from room temperature to 650 deg.C at a heating rate of 2 deg.C/min under nitrogen atmosphere, maintaining for 2 hr, and cooling to room temperature at a cooling rate of 10 deg.C/min to obtain Co/CoSe/MoSe 2 A composite material. FIG. 1 shows Co/CoSe/MoSe 2 Comparison of XRD with standard card, with standard card (JCPDs MoSe) 2 No. 04-6645), (JCPDs CoSe No. 89-2004), and (JCPDs Co No. 89-4307), and showed good crystallinity without significant peaks. But no obvious carbon peak appears, which indicates that the compounded carbon is amorphous carbon. FIG. 2 is Co/CoSe/MoSe 2 The SEM image of (1) shows that the material is in a submicron rod structure, the diameter of the submicron rod is about 200 nm, the length of the submicron rod is 3-4 mu m, the surface of the submicron rod is smooth, and the submicron rod and the carbon material are uniformly compounded. FIG. 3 is Co/CoSe/MoSe 2 At 0.1, 0.2, 0.5, 1, 2 and 5A g -1 Rate performance diagram under current density, as negative electrode material of sodium ion battery, 0.1A g -1 The capacity is stabilized at 400 mAh g under the current density -1 And at 5A g -1 Still has 273.5 mAh g under the current density -1 The specific capacity of the electrolyte shows excellent electrochemical performance. FIG. 4 is Co/CoSe/MoSe 2 The first three circles of charge and discharge performance graphs show that the discharge specific capacity of the first circle reaches 536.6 mAh g -1 The first coulombic efficiency was 72.13% due to the irreversible capacity fading caused by the SEI film formation. The material tends to be stable from the second circle, and the specific discharge capacity is stable at 400 mAh g -1 This is consistent with the graph of the rate performance.
Example 2
Adding 7 mmol of Co (CH) 3 COO) 2 ·4H 2 O、1 mmol (NH 4 ) 6 Mo 7 O 24 ·4H 2 Placing O in a beaker, adding 50 mL of deionized water, stirring for 4 h at 50 ℃, centrifuging at 4000 rpm to obtain cobalt molybdate, and placing in an oven to dry for 12 h at 60 ℃. Dispersing 2 mmol of cobalt molybdate in 4 mL of DMF solution, then adding 0.3 g of PAN, 0.1g of PVP and 4 mmol of selenium powder, and stirring uniformly to obtain the electrostatic spinning precursor dispersion liquid. The dispersion was transferred to a syringe and the syringe was mounted on a micropump syringe, the positive pole being connected to the syringe needle and the negative pole to the collector. The distance between the anode and the cathode is 17 cm, the voltage of the anode is 16.5 kV, the voltage of the cathode is-2.5 kV, the sample injection speed of the micro pump is 1mL/h, and the temperature of the equipment is 30 ℃ The fibrous mixture is then collected on a collector. Peeling the fibrous mixture from the collector, drying at 80 deg.C for 24 hr in an oven, transferring to a tubular furnace, heating from room temperature to 650 deg.C at a heating rate of 2 deg.C/min under nitrogen atmosphere, maintaining for 2 hr, and cooling to room temperature at a cooling rate of 10 deg.C/min to obtain Co/MoSe 2 . FIG. 1 is Co/MoSe 2 Comparison of XRD with standard card, with standard card (JCPDs MoSe) 2 No.04-6645, and JCPDs Co No. 89-4307), no obvious hetero peak, and good crystallinity. But no obvious carbon peak appears, which indicates that the compounded carbon is amorphous carbon. FIG. 3 is Co/MoSe 2 At 0.1, 0.2, 0.5, 1, 2 and 5A g -1 Rate performance diagram under current density, as negative electrode material of sodium ion battery, 0.1A g -1 The capacity is stabilized at 348 mAh g under the current density -1 And at 5A g -1 173.3 mAh g at current density -1 The specific capacity of the electrolyte shows good electrochemical performance. FIG. 5 is Co/MoSe 2 The first three circles of charge-discharge performance graphs show that the first circle of discharge specific capacity reaches 501.3 mAh g -1 The first coulombic efficiency was 68.16% due to the irreversible capacity fading caused by the SEI film formation. The material tends to be stable from the second circle, and the specific discharge capacity is stabilized at 348 mAh g -1 This is consistent with the graph of the rate performance.
Example 3
Dispersing 2 mmol of molybdenum trioxide in 4 mL of DMF solution, then adding 0.3 g of PAN, 0.1g of PVP and 4 mmol of selenium powder, and uniformly stirring to obtain the electrostatic spinning precursor dispersion liquid. The dispersion was transferred to a syringe and the syringe was fixed to a micro-pump injector, the positive electrode was connected to the syringe needle and the negative electrode to the collector. The distance between the positive and negative electrodes was made 17 cm, the positive electrode voltage was 16.5 kV, the negative electrode voltage was-2.5 kV, the sample injection speed of the micro pump was 1mL/h, the temperature of the apparatus was 30 ℃, and then the fibrous mixture was collected on a collector. Peeling the fibrous mixture from the collector, drying at 80 ℃ for 24 h in an oven, transferring to a tube furnace, heating to 650 ℃ from room temperature at a heating rate of 2 ℃/min under nitrogen atmosphere, keeping the temperature for 2 h, and then cooling to room temperature at a cooling rate of 10 ℃/min to obtain molybdenum diselenide named MoSe 2 . FIG. 1 is MoSe 2 Comparison of XRD with standard card, with standard card (JCPDs MoSe) 2 No. 04-6645) and a small amount of hetero-peaks presumed to be MoO x . But no obvious carbon peak appears, which indicates that the compounded carbon is amorphous carbon. FIG. 3 is MoSe 2 At 0.1, 0.2, 0.5, 1, 2 and 5A g -1 Rate performance diagram under current density, as negative electrode material of sodium ion battery, 0.1A g -1 The discharge capacity is stabilized at 264 mAh g under the current density -1 And at 5A g -1 Only 125 mAh g under the current density -1 The specific capacity of the electrolyte shows poor electrochemical performance. FIG. 6 is MoSe 2 The first three circles of charge-discharge performance graphs show that the first circle of discharge specific capacity reaches 401.8 mAh g -1 The first coulombic efficiency was 69.32% due to the irreversible capacity fading caused by the SEI film formation. The material tends to be stable from the second circle, and the specific discharge capacity is stabilized at 264 mAh g -1 Left and right, consistent with the magnification performance graph.
Example 4
In the same manner as in example 1, Co/CoSe/MoSe was obtained by adjusting the distance between the positive and negative electrodes to 42cm, the positive electrode voltage to 25 kV and the negative electrode voltage to-5 kV 2 。Co/CoSe/MoSe 2 As a negative electrode material of sodium ion battery, 0.1A g -1 The capacity is stabilized at 310mAh g under the current density -1 And at 5A g -1 Still has 101 mAh g under the current density -1 The specific capacity of the composite material shows excellent electrochemical performance. Co/CoSe/MoSe 2 The first circle of discharge specific capacity in the first three circles of charge and discharge performance reaches 320 mAh g -1 The first coulombic efficiency was 52.12% due to the irreversible capacity fading caused by the SEI film formation. The material tends to be stable from the second circle, and the specific discharge capacity is stabilized at 220 mAh g -1 。
Example 5
In the same manner as in example 1, the distance between the positive electrode and the negative electrode was set to 17 cm, the voltage of the positive electrode was set to 18kV, and the voltage of the negative electrode was set to-0.5 kV, to obtain Co/CoSe/MoSe 2 。Co/CoSe/MoSe 2 As a negative electrode material of sodium ion battery, 0.1A g -1 The capacity is stabilized at 380mAh g under the current density -1 And at 5A g -1 Still has 82 mAh g under the current density -1 The specific capacity of the electrolyte shows excellent electrochemical performance. Co/CoSe/MoSe 2 The first circle of discharge specific capacity in the first three circles of charge and discharge performance reaches 290mAh g -1 The first coulombic efficiency was 53.26% due to the irreversible capacity fading caused by the SEI film formation. The material tends to be stable from the second circle, and the specific discharge capacity is stable at 200mAh g -1 。
Claims (10)
1. A kind ofCo/CoSe/MoSe 2 The preparation method of the composite material is characterized by comprising the following steps:
the method comprises the following steps: preparing a mixed solution from cobalt acetate and ammonium molybdate according to a proportion, forming cobalt molybdate by a coprecipitation method, drying, adding the cobalt molybdate into a DMF solution, then adding a proper amount of PAN, PVP and selenium powder, and uniformly stirring to obtain a precursor dispersion liquid;
step two: transferring the precursor dispersion liquid in the step one into an injector, fixing the injector on a micro-pump injector, connecting a positive electrode with a syringe needle, connecting a negative electrode with a collector, and collecting a fibrous mixture on the collector by adjusting the distance between the positive electrode and the negative electrode, the voltage of the positive electrode and the negative electrode, the sample injection speed of the micro-pump and the temperature of equipment;
step three: drying the fibrous mixture in the second step, peeling off the fibrous mixture from a collector, transferring the fibrous mixture to a tube furnace, and selenizing the fibrous mixture at high temperature in an inert atmosphere to obtain Co/CoSe/MoSe 2 A composite material.
2. Co/CoSe/MoSe as claimed in claim 1 2 The preparation method of the composite material is characterized by comprising the following steps:
in the first step, the molar ratio of the cobalt acetate to the ammonium molybdate is 1-2: 0.1-0.3, the temperature in the drying process is 40-100 ℃, and the drying time is 10-24 h.
3. Co/CoSe/MoSe as claimed in claim 1 2 The preparation method of the composite material is characterized by comprising the following steps: when preparing the electrostatic spinning mixed solution in the first step, the molar ratio of cobalt molybdate to selenium powder is 1-3: 2-10; the mass concentrations of PAN and PVP in the precursor dispersion liquid are 0.01-0.1g/mL and 0.01-0.05g/mL respectively.
4. Co/CoSe/MoSe as claimed in claim 1 2 The preparation method of the composite material is characterized by comprising the following steps: in the second step, the distance between the needle connected with the anode and the collector connected with the cathode is 10-40 cm.
5. C as claimed in claim 1o/CoSe/MoSe 2 The preparation method of the composite material is characterized by comprising the following steps: in the second step, the voltage of the positive electrode is 10-30 kV, and the voltage of the negative electrode is 1-10 kV.
6. Co/CoSe/MoSe as claimed in claim 1 2 The preparation method of the composite material is characterized by comprising the following steps: and in the second step, the sample injection speed of the micro pump is 0.1-4 mL/h.
7. Co/CoSe/MoSe as claimed in claim 1 2 The preparation method of the composite material is characterized by comprising the following steps: in the second step, the temperature of the electrostatic spinning equipment is maintained at 10-60 ℃.
8. Co/CoSe/MoSe as claimed in claim 1 2 The preparation method of the composite material is characterized by comprising the following steps: in the third step, the drying temperature of the fibrous mixture is 60-100 ℃, and the drying time is 10-48 h.
9. Cobalt Co/CoSe/MoSe as claimed in claim 1 2 The preparation method of the composite material is characterized by comprising the following steps: the inert gas in the third step is one of nitrogen, argon or the mixture of the nitrogen and the argon.
10. Co/CoSe/MoSe as claimed in claim 1 2 The preparation method of the composite material is characterized by comprising the following steps: the conditions of high-temperature selenization in the third step are as follows: raising the temperature from room temperature to 400-800 ℃ at the speed of 1-10 ℃/min, preserving the temperature for 1-4 h, and finally reducing the temperature to room temperature at the speed of 1-10 ℃/min.
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