CN114583129B - Sodium vanadate/molybdenum disulfide nanobelt composite material, preparation method thereof and application thereof in magnesium ion battery - Google Patents

Sodium vanadate/molybdenum disulfide nanobelt composite material, preparation method thereof and application thereof in magnesium ion battery Download PDF

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CN114583129B
CN114583129B CN202210216714.0A CN202210216714A CN114583129B CN 114583129 B CN114583129 B CN 114583129B CN 202210216714 A CN202210216714 A CN 202210216714A CN 114583129 B CN114583129 B CN 114583129B
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sodium vanadate
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molybdenum disulfide
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CN114583129A (en
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韩阗俐
王程杨
林夕蓉
陈中华
龙佳炜
朱亚军
刘金云
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Anhui Normal University
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Abstract

The invention discloses a sodium vanadate/molybdenum disulfide nanobelt composite material, a preparation method and application thereof in a magnesium ion battery, wherein sodium vanadate nanobelt is obtained through simple stirring, and then is mixed with a molybdenum source, a sulfur source and polyethylene glycol 750 monomethyl ether for hydrothermal growth to obtain the molybdenum disulfide coated sodium vanadate nanobelt composite material.

Description

Sodium vanadate/molybdenum disulfide nanobelt composite material, preparation method thereof and application thereof in magnesium ion battery
Technical Field
The invention belongs to the technical field of inorganic nano materials, and particularly relates to a sodium vanadate/molybdenum disulfide nanobelt composite material, a preparation method thereof and application thereof in a magnesium ion battery.
Background
Due to the low cost, high natural storage and high volume capacity (3833 mA h cm) -3 ) Magnesium ion batteries are one of the promising candidate batteries other than lithium ion batteries. More importantly, the magnesium metal cathode does not generate dendrites during electrochemical deposition, which basically ensures high safety for large-scale application. In addition, the use of metallic magnesium cathodes greatly broadens the potential choice of cathode materials, as more magnesium-deficient cathode materials can be selected. So far, research into magnesium ion batteries is still in the preliminary stage. Magnesium ion batteries face two major obstacles in practical applications: 1) Intercalation diffusion kinetics of magnesium ions in the positive electrode material is slow; 2) Divalent magnesium ions have a high polarizability, resulting in incompatibility of the anode with the electrolyte.
The positive electrode material disclosed in the prior art mainly comprises: cobalt-based positive electrodes, molybdenum-based positive electrodes, manganese-based positive electrodes, and the like, which generally exhibit low capacity, poor kinetics, and poor reversibility of magnesium storage.
Disclosure of Invention
In order to solve the technical problems, the invention provides a sodium vanadate/molybdenum disulfide nanobelt composite material and a preparation method thereof, wherein sodium vanadate nanobelt is obtained through simple stirring, and then the sodium vanadate nanobelt composite material is obtained through hydrothermal growth by mixing the sodium vanadate nanobelt with a molybdenum source, a sulfur source and polyethylene glycol 750 monomethyl ether, and the preparation method is simple.
The invention also provides a magnesium ion battery anode and a magnesium ion battery, wherein the magnesium ion battery anode is prepared by taking the sodium vanadate/molybdenum disulfide nanobelt composite material as an active substance, and the magnesium ion battery is further assembled by taking the sodium vanadate/molybdenum disulfide nanobelt composite material as the anode.
In order to achieve the above purpose, the technical scheme adopted by the invention is as follows:
the preparation method of the sodium vanadate/molybdenum disulfide nanobelt composite material comprises the following steps:
(1) Dissolving a vanadium source and a sodium source in deionized water, stirring for reaction, performing ultrasonic treatment, centrifugally washing and drying the product to obtain a sodium vanadate nanobelt;
(2) Dissolving a molybdenum source and a sulfur source in deionized water, adding polyethylene glycol 750 monomethyl ether into the solution, stirring and dissolving the solution, ultrasonically dispersing the sodium vanadate nanobelt prepared in the step (1) into the solution, performing a hydrothermal reaction, and washing and drying the obtained product to obtain the sodium vanadate/molybdenum disulfide nanobelt composite material.
In the step (1), the vanadium source is any one or more of vanadium pentoxide, vanadium tetraoxide and vanadium trioxide; the sodium source is any one or more of sodium chloride, sodium carbonate and sodium bicarbonate.
In the step (1), the stirring reaction condition is that stirring reaction is carried out for 12-120 hours at 20-38 ℃, preferably stirring reaction is carried out for 60-84 hours at 27-33 ℃; the condition of the ultrasonic treatment is that the ultrasonic treatment is carried out for 20-120 min at 25-45 ℃, and the ultrasonic treatment is carried out for 30-90 min at 25-35 ℃ preferably.
In the step (1), the mass ratio of the vanadium source to the sodium source is 1: 1.5-5.0 g; the concentration of the vanadium source in deionized water is 0.01-0.15 g/mL.
In the step (2), the molybdenum source is one or two of ammonium molybdate and sodium molybdate; the sulfur source is any one or more of thioacetamide, thiourea, L-cysteine and sodium sulfide.
In the step (2), the hydrothermal reaction condition is 120-240 ℃ for 1-24 hours, preferably 160-200 ℃ for 3-6 hours.
In the step (2), the mass ratio of the molybdenum source, the sulfur source, the polyethylene glycol 750 monomethyl ether and the sodium vanadate nanobelt is 1:0.3 to 1.5:0.2 to 1.5:0.1 to 1.0; the concentration of the molybdenum source in deionized water is 0.01-1.0g/mL.
The sodium vanadate/molybdenum disulfide nanobelt composite material prepared by the preparation method disclosed by the invention has the advantages that molybdenum disulfide is wrapped on the surface of the sodium vanadate nanobelt, so that a porous lamellar structure is formed.
The magnesium ion battery anode provided by the invention is prepared by taking the sodium vanadate/molybdenum disulfide nanobelt composite material as an active substance.
The magnesium ion battery provided by the invention is assembled by taking the positive electrode of the magnesium ion battery as the positive electrode.
According to the invention, a vanadium source and a sodium source are dissolved in deionized water, and sodium vanadate nanobelt is obtained through simple stirring reaction and ultrasonic treatment. Dissolving a molybdenum source and a sulfur source in ionized water, adding polyethylene glycol 750 monomethyl ether into the solution, stirring the solution, adding sodium vanadate nanobelt, carrying out ultrasonic treatment, transferring the compound into a stainless steel reaction kettle for hydrothermal reaction, and collecting, washing and drying the obtained compound product to obtain a sodium vanadate/molybdenum disulfide nanobelt compound material product which has a porous lamellar structure. The porous lamellar skeleton is favorable for rapid movement of ions, has higher specific capacity in a magnesium ion battery, and sodium ions contained in the product sodium vanadate/molybdenum disulfide nanobelt composite material can weaken strong interaction between magnesium ions and host sodium metavanadate lattices, so that the electrochemical performance of the magnesium ions is further improved. The molybdenum disulfide in the sodium vanadate/molybdenum disulfide nanobelt composite material has a structure similar to graphene, two sulfur atoms and one molybdenum atom are overlapped together by virtue of weak van der Waals interaction, the special structure is favorable for embedding and extracting magnesium ions, and the magnesium ion battery anode prepared by taking the sodium vanadate/molybdenum disulfide nanobelt composite material as an active substance is used as the magnesium ion anode, so that the magnesium ion battery has the advantages of good cycle performance, stability and high specific capacity.
Compared with the prior art, the invention has the following advantages:
(1) The synthesis process is simple, the device is convenient and reliable, the raw materials are easy to obtain, the cost is low, and the mass production can be realized.
(2) The synthesis process is environment-friendly, has no toxic and harmful pollutant generation, and is suitable for industrial production.
(3) The composite material has stable performance, is not easy to be changed in air and is easy to store.
(4) The composite material has the structural characteristics of two materials, namely sodium vanadate and molybdenum disulfide, is convenient for embedding and extracting magnesium ions, and greatly improves the cycling stability and specific capacity of the magnesium ion battery.
Drawings
FIG. 1 is an SEM image of sodium vanadate nanoribbons prepared in example 1;
FIG. 2 is an SEM image of the sodium vanadate/molybdenum disulfide nanobelt composite prepared in example 1;
FIG. 3 is an SEM image of sodium vanadate nanoribbons prepared in example 2;
FIG. 4 is an SEM image of the sodium vanadate/molybdenum disulfide nanobelt composite prepared in example 2;
FIG. 5 is an SEM image of sodium vanadate nanoribbons prepared in example 3;
FIG. 6 is an SEM image of a sodium vanadate/molybdenum disulfide nanobelt composite prepared in example 3;
FIG. 7 is an SEM image of sodium vanadate nanoribbons prepared in example 4;
FIG. 8 is an SEM image of a sodium vanadate/molybdenum disulfide nanobelt composite prepared in example 4;
FIG. 9 is an SEM image of sodium vanadate nanoribbons prepared in example 5;
FIG. 10 is an SEM image of a sodium vanadate/molybdenum disulfide nanobelt composite prepared in example 5;
FIG. 11 is a TEM image of sodium vanadate nanoribbons prepared in example 5;
FIG. 12 is a TEM image of the sodium vanadate/molybdenum disulfide nanobelt composite prepared in example 5;
FIG. 13 is a HRTEM image of the sodium vanadate/molybdenum disulfide nanobelt composite prepared in example 5;
FIG. 14 is a SAED pattern of the sodium vanadate/molybdenum disulfide nanobelt composite material prepared in example 5;
FIG. 15 is an XRD pattern of sodium vanadate nanoribbons prepared in example 5;
FIG. 16 is an XRD pattern of the sodium vanadate/molybdenum disulfide nanobelt composite prepared in example 5;
FIG. 17 is an XPS full spectrum of the sodium vanadate/molybdenum disulfide nanobelt composite prepared in example 5;
FIG. 18 is a high resolution XPS spectrum of Na 1s of the sodium vanadate/molybdenum disulfide nanobelt composite prepared in example 5;
FIG. 19 is a high resolution XPS spectrum of V2 p of the sodium vanadate/molybdenum disulfide nanobelt composite prepared in example 5;
FIG. 20 is a high resolution XPS spectrum of O1s of the sodium vanadate/molybdenum disulfide nanobelt composite prepared in example 5;
FIG. 21 is a high resolution XPS spectrum of Mo 3d of the sodium vanadate/molybdenum disulfide nanobelt composite prepared in example 5;
FIG. 22 is a high resolution XPS spectrum of S2 p of the sodium vanadate/molybdenum disulfide nanobelt composite prepared in example 5;
FIG. 23 is a Mapping graph of each element of the sodium vanadate/molybdenum disulfide nanobelt composite prepared in example 5;
FIG. 24 is a CV graph of the sodium vanadate/molybdenum disulfide nanobelt composite prepared in example 5 as a magnesium ion battery positive electrode material tested at 0.1m V/s;
FIG. 25 is a charge-discharge graph of the sodium vanadate/molybdenum disulfide nanobelt composite prepared in example 5 as a magnesium ion battery cathode material;
FIG. 26 is a graph showing the cycling performance of the sodium vanadate/molybdenum disulfide nanobelt composite prepared in example 5 as a magnesium ion battery positive electrode material at a current density of 50 mA/g;
FIG. 27 is an impedance spectrum of the sodium vanadate/molybdenum disulfide nanobelt composite prepared in example 5 as a magnesium ion battery cathode material.
Detailed Description
The present invention will be described in detail with reference to examples.
Example 1
The preparation method of the sodium vanadate/molybdenum disulfide nanobelt composite material comprises the following steps:
1) Preparation of sodium vanadate nanobelts: placing 1.0g of vanadium pentoxide and 4.3875g of sodium chloride into a 250mL beaker, adding 75mL of ultrapure water, stirring for 12 hours at a constant temperature of 25 ℃, carrying out ultrasonic treatment on the suspension for 1 hour after stirring, alternately washing 3 times with distilled water and ethanol, centrifugally collecting a product, and drying at 60 ℃ for 24 hours to obtain a sodium vanadate nanobelt product, wherein an SEM (scanning electron microscope) diagram is shown in figure 1;
2) Preparation of sodium vanadate/molybdenum disulfide nanobelt composite material: placing 0.392g of ammonium molybdate and 0.3757g of thioacetamide into a 100mL beaker, adding 30mL of pure water, stirring and dissolving, adding 0.3g of polyethylene glycol monomethyl ether into the mixed solution, stirring for 1h, adding 0.2g of sodium vanadate nanobelt into the mixed solution, carrying out ultrasonic treatment for 20min, transferring the mixed suspension into a reaction kettle, reacting at 120 ℃ in a blast drying box for 1h, taking out a sample after cooling to room temperature, washing with ultrapure water for several times, centrifugally collecting the product, and placing the product into a vacuum drying box for drying at 70 ℃ overnight to obtain the product sodium vanadate/molybdenum disulfide nanobelt composite material which is molybdenum disulfide-coated sodium vanadate nanobelt, wherein an SEM (SEM) graph of the product is shown in figure 2.
Example 2
The preparation method of the sodium vanadate/molybdenum disulfide nanobelt composite material comprises the following steps:
1) Preparation of sodium vanadate nanobelts: placing 3.0g of vanadium pentoxide and 13.1625g of sodium chloride into a 250mL beaker, adding 75mL of ultrapure water, stirring for 24 hours at a constant temperature of 25 ℃, carrying out ultrasonic treatment on the suspension for 1 hour after stirring, alternately washing 3 times with distilled water and ethanol, centrifugally collecting a product, and drying at 60 ℃ for 24 hours to obtain a sodium vanadate nanobelt product, wherein an SEM (scanning electron microscope) diagram is shown in figure 3;
2) Preparation of sodium vanadate/molybdenum disulfide nanobelt composite material: placing 0.865g of ammonium molybdate and 0.3381g of thioacetamide into a 100mL beaker, adding 30mL of pure water, stirring and dissolving, adding 0.5g of polyethylene glycol monomethyl ether into the mixed solution, stirring for 1h, adding 0.2g of sodium vanadate nanobelt into the mixed solution, carrying out ultrasonic treatment for 20min, transferring the mixed suspension into a reaction kettle, reacting for 1h at 180 ℃ in a blast drying box, taking out a sample after cooling to room temperature, washing with ultrapure water for several times, centrifugally collecting the product, and placing in a vacuum drying box and drying overnight at 70 ℃ to obtain the product sodium vanadate/molybdenum disulfide nanobelt composite material, wherein the product is molybdenum disulfide-coated sodium vanadate nanobelt, and an SEM (SEM) graph of the product is shown in figure 4.
Example 3
The preparation method of the sodium vanadate/molybdenum disulfide nanobelt composite material comprises the following steps:
1) Preparation of sodium vanadate nanobelts: placing 4.0g of vanadium pentoxide and 17.55g of sodium chloride into a 250mL beaker, adding 75mL of ultrapure water, stirring for 36 hours at a constant temperature of 25 ℃, carrying out ultrasonic treatment on the suspension for 1 hour after stirring, alternately washing 3 times with distilled water and ethanol, centrifuging to collect a product, and drying at 60 ℃ for 24 hours to obtain a sodium vanadate nanobelt product, wherein an SEM (scanning electron microscope) diagram is shown in figure 5;
2) Preparation of sodium vanadate/molybdenum disulfide nanobelt composite material: 1.764g of ammonium molybdate and 1.3523g of thioacetamide are placed in a 100mL beaker, 30mL of pure water is added for stirring and dissolution, 0.5g of polyethylene glycol monomethyl ether is added into the mixed solution, stirring is carried out for 1h, 0.2g of sodium vanadate nanobelt is added into the mixed solution, ultrasound is carried out for 20min, the mixed suspension is transferred into a reaction kettle, and reaction is carried out for 12h at 180 ℃ in a blast drying box. And taking out the sample after cooling to room temperature, washing the sample with ultrapure water for a plurality of times, centrifugally collecting the product, and placing the product in a vacuum drying oven for drying at 70 ℃ overnight to obtain the product sodium vanadate/molybdenum disulfide nanobelt composite material, wherein the product is molybdenum disulfide coated sodium vanadate nanobelt, and an SEM (scanning electron microscope) diagram of the product is shown in figure 6.
Example 4
The preparation method of the sodium vanadate/molybdenum disulfide nanobelt composite material comprises the following steps:
1) Preparation of sodium vanadate nanobelts: placing 8.0g of vanadium pentoxide and 21.9375g of sodium chloride into a 250mL beaker, adding 75mL of ultrapure water, stirring for 72 hours at a constant temperature of 25 ℃, carrying out ultrasonic treatment on the suspension for 1 hour after stirring, alternately washing 3 times with distilled water and ethanol, centrifugally collecting a product, and drying at 60 ℃ for 24 hours to obtain a sodium vanadate nanobelt product, wherein an SEM (scanning electron microscope) diagram is shown in FIG. 7;
2) Preparation of sodium vanadate/molybdenum disulfide nanobelt composite material: placing 0.865g of ammonium molybdate and 1.0143g of thioacetamide into a 100mL beaker, adding 30mL of pure water, stirring and dissolving, adding 1g of polyethylene glycol monomethyl ether into the mixed solution, stirring for 1h, adding 0.2g of sodium vanadate nanobelt into the mixed solution, carrying out ultrasonic treatment for 20 minutes, transferring the mixed suspension into a reaction kettle, reacting at 200 ℃ in a blast drying box for 6h, taking out a sample after cooling to room temperature, washing with ultrapure water for several times, centrifuging to collect a product, and placing the product into a vacuum drying box for drying at 70 ℃ overnight to obtain a product sodium vanadate/molybdenum disulfide nanobelt composite material, wherein the product is molybdenum disulfide-coated sodium vanadate nanobelt, and an SEM (SEM) graph of the product is shown in figure 8.
Example 5
The preparation method of the sodium vanadate/molybdenum disulfide nanobelt composite material comprises the following steps:
1) Preparation of sodium vanadate nanobelts: placing 5.0g of vanadium pentoxide and 8.775g of sodium chloride into a 250mL beaker, adding 75mL of ultrapure water, stirring for 72 hours at a constant temperature of 25 ℃, carrying out ultrasonic treatment on the suspension for 1 hour after stirring, alternately washing with distilled water and ethanol for 3 times, centrifugally collecting the product, and drying at 60 ℃ for 24 hours to obtain a sodium vanadate nanobelt product, wherein an SEM (scanning electron microscope) graph is shown in FIG. 9, a TEM (transmission electron microscope) graph is shown in FIG. 10, and an XRD (X-ray diffraction) graph is shown in FIG. 15;
2) Preparation of sodium vanadate/molybdenum disulfide nanobelt composite material: placing 0.865g of ammonium molybdate and 0.87g of thioacetamide into a 100mL beaker, adding 30mL of pure water, stirring and dissolving, adding 0.5g of polyethylene glycol monomethyl ether into the mixed solution, stirring for 1h, adding 0.2g of sodium vanadate nanobelt into the mixed solution, carrying out ultrasonic treatment for 20min, transferring the mixed suspension into a reaction kettle, reacting for 3h at 180 ℃ in a blast drying box, taking out a sample after cooling to room temperature, washing with ultrapure water for several times, centrifugally collecting the product, and placing the product into a vacuum drying box for drying at 70 ℃ overnight to obtain the product sodium vanadate/molybdenum disulfide nanobelt composite material, wherein the product sodium vanadate nanobelt is wrapped by molybdenum disulfide, the SEM graph is shown in FIG. 10, the TEM graph is shown in FIG. 13, the SAED graph is shown in FIG. 14, the XRD graph is shown in FIG. 16, the XPS full spectrum is shown in FIG. 17, and the XPS graphs of each element are shown in FIG. 18-22 respectively. The Mapping diagram of each element is shown in fig. 23.
As can be seen from fig. 10, 12, 13 and 16-22, the sodium vanadate/molybdenum disulfide nanobelt composite material prepared in the embodiment is a sodium vanadate nanobelt wrapped by molybdenum disulfide.
The prepared sodium vanadate/molybdenum disulfide nanobelt composite material is a polycrystalline material from the multi-ring in fig. 14.
From the Mapping graph of the elements of fig. 23, a uniform distribution of sodium, vanadium, oxygen, molybdenum and sulfur elements can be observed, demonstrating the success of the compounding of sodium vanadate and molybdenum disulfide materials. Meanwhile, the color display of molybdenum and sulfur elements is clearer, and the color display of sodium, vanadium and oxygen elements is relatively weaker, so that the sodium vanadate is shown in the inner layer, the molybdenum disulfide is shown in the outer layer, and the molybdenum disulfide successfully wraps the sodium vanadate.
Application example 1
Application of sodium vanadate/molybdenum disulfide nanobelt composite material in magnesium ion battery
The final product sodium vanadate/molybdenum disulfide nanobelt composite material obtained in the step B of the example 5 is mixed with conductive carbon black and PVDF in a mass ratio of 80:10:10 in N-methyl pyrrolidone (NMP) solvent to prepare uniform slurry, coating the slurry on 304 stainless steel foil, and drying at 60 ℃ in vacuum for 24 hours. The dried electrode slice is subjected to tabletting treatment by a pair roller machine or a tablet press, and then is cut by a mechanical cutting machine to obtain round electrode slices with uniform size, wherein the round electrode slices are used as positive electrodes, high-purity Mg slices are used as counter electrodes, glass fibers are used as diaphragms, and 0.4M (PhMgCl) 2 -AlCl 3 THF (APC) was used as electrolyte. The CR2032 type battery was assembled in a glove box.
The charge and discharge performance test is carried out by using a battery tester, the CV curve of the magnesium ion battery at the front 6 circles is measured in the voltage range of 0-2.0V and the sweeping speed of 0.1m V/s, as shown in the figure 24, and the battery has good cycle stability. As can be seen from the constant current charge-discharge curve of FIG. 25, the battery capacity is still stable at 100mAh/g after 100 cycles. The cycling performance is shown in FIG. 26, and the capacity is stabilized at 70mAh/g after cycling 100 times at a current density of 50 mA/g. Fig. 27 is a graph of battery impedance testing showing the stability of the resistance of the battery after 100 cycles.
The foregoing detailed description of a sodium vanadate/molybdenum disulfide nanobelt composite, and methods for its preparation and its use in magnesium ion batteries is illustrative and not limiting. Several embodiments may be enumerated in accordance with the defined scope, and therefore variations and modifications may be resorted to without departing from the general inventive concept.

Claims (10)

1. The preparation method of the sodium vanadate/molybdenum disulfide nanobelt composite material is characterized by comprising the following steps of:
(1) Dissolving a vanadium source and a sodium source in deionized water, stirring for reaction, performing ultrasonic treatment, centrifugally washing and drying the product to obtain a sodium vanadate nanobelt;
(2) Dissolving a molybdenum source and a sulfur source in deionized water, adding polyethylene glycol 750 monomethyl ether into the solution, stirring and dissolving the solution, ultrasonically dispersing the sodium vanadate nanobelt prepared in the step (1) into the solution, performing a hydrothermal reaction, and washing and drying the obtained product to obtain the sodium vanadate/molybdenum disulfide nanobelt composite material.
2. The method according to claim 1, wherein in the step (1), the vanadium source is any one or more of vanadium pentoxide, vanadium tetraoxide and vanadium trioxide; the sodium source is any one or more of sodium chloride, sodium carbonate and sodium bicarbonate.
3. The method according to claim 1, wherein in the step (1), the condition of the stirring reaction is 20-38 ℃ for stirring reaction for 12-120 hours; the condition of the ultrasonic treatment is that the ultrasonic treatment is carried out for 20-120 min at 25-45 ℃.
4. The preparation method according to claim 1, wherein in the step (1), the mass ratio of the vanadium source to the sodium source is 1: 1.5-5.0 g; the concentration of the vanadium source in deionized water is 0.01-0.15 g/mL.
5. The method according to claim 1, wherein in the step (2), the molybdenum source is one or both of ammonium molybdate and sodium molybdate; the sulfur source is any one or more of thioacetamide, thiourea, L-cysteine and sodium sulfide.
6. The method according to claim 1, wherein in the step (2), the hydrothermal reaction is carried out at 120 to 240 ℃ for 1 to 24 hours.
7. The preparation method of claim 1, wherein in the step (2), the mass ratio of the molybdenum source, the sulfur source, the polyethylene glycol 750 monomethyl ether and the sodium vanadate nanobelt is 1:0.3 to 1.5:0.2 to 1.5:0.1 to 1.0; the concentration of the molybdenum source in deionized water is 0.01-1.0g/mL.
8. The sodium vanadate/molybdenum disulfide nanobelt composite material prepared by the preparation method of any one of claims 1-7.
9. The magnesium ion battery anode is characterized in that the magnesium ion battery anode is prepared by taking the sodium vanadate/molybdenum disulfide nanobelt composite material as an active substance.
10. A magnesium ion battery, wherein the positive electrode of the magnesium ion battery according to claim 9 is used as a positive electrode.
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