CN111320207A - Preparation and application of molybdenum sulfide material - Google Patents
Preparation and application of molybdenum sulfide material Download PDFInfo
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Abstract
The invention belongs to the field of inorganic chemical nano materials and related electrochemical technologies, and relates to a preparation method of a molybdenum disulfide material and a general method of the molybdenum disulfide material in application of an aluminum ion battery anode. According to the invention, a molybdenum disulfide precursor is obtained by using a microwave treatment method, and then the molybdenum disulfide precursor is synthesized by combining a high-temperature calcination crystallization method, and the morphology and size of the synthesized molybdenum disulfide are controlled by controlling the microwave treatment power and time, so that the high-performance aluminum ion battery anode material is obtained. The discharge specific capacity of the lithium ion battery is still higher under higher current density, which shows that the lithium ion battery has very great application prospect as a large-capacity aluminum ion battery anode active material. Meanwhile, as the raw materials such as sodium molybdate, thiourea and the like are used, the source is wide, the price is low, the preparation process of the electrode material is simple and controllable, the condition is mild, the equipment is simple, and the method is easy for large-scale production.
Description
Technical Field
The invention relates to preparation of a molybdenum disulfide material and application of the molybdenum disulfide material as an aluminum ion battery anode, and belongs to the field of inorganic nano materials and electrochemistry.
Background
The aluminum ion battery is a novel chargeable and dischargeable battery based on transmission of aluminum ions between a positive electrode and a negative electrode, and the aluminum negative electrode has the characteristics of high capacity, good safety, wide source and low price; meanwhile, the aluminum ion battery has the characteristics of long cycle life, quick charge and slow discharge, wide working temperature range and the like. Based on the advantages, the aluminum ion battery is expected to become a main energy supply device of portable electronic products such as mobile phones, cameras and notebook computers in the future, and is very likely to be applied to future products such as power automobiles and portable wearable electronic equipment. Therefore, the research on the aluminum ion battery and the electrode material thereof is receiving increasing attention.
At present, the anode materials of the aluminum ion batteries which are widely researched mainly comprise carbon materials including reduced graphene oxide, graphite and the like, but the carbon materials are limited by low theoretical capacity of the carbon materials; the other is transition metal oxide, such as vanadium pentoxide, copper oxide and the like, which has high theoretical specific capacity, but the application of the transition metal oxide is limited by poor conductivity, poor cycling stability, low discharge voltage platform and the like; there are also some two-dimensional graphene-like materials, such as nickel sulfide, tin sulfide, etc., which also have disadvantages of poor conductivity, poor structural stability, etc. Therefore, the search for positive electrode materials with high energy density and good cycle stability and conductivity is the focus of research in current aluminum ion batteries. The common methods adopted by the conventional aluminum ion battery anode material exploration and modification research comprise a compounding method, such as compounding a carbon material, a transition metal oxide and a transition metal sulfide to increase the specific surface area of the material and enhance the conductivity and the cycle stability; morphology control and particle size control are also common methods to enhance the dynamic properties of materials by synthesizing specific morphologies such as hierarchical pore structures.
At present, researches on transition metal sulfide type aluminum ion battery anode materials mainly focus on preparing materials with high specific surface area, porous structures, smaller internal resistance, high conductivity, high cost performance, good cycle stability and special structures. Among various transition metal sulfides, molybdenum disulfide has the characteristics of high theoretical capacity, simple synthesis process, low price and the like, and is an ideal aluminum ion battery anode material candidate.
Disclosure of Invention
The invention aims to avoid the defects of the prior art and provides a molybdenum disulfide aluminum ion battery anode material and a preparation method thereof.
The preparation method comprises the following specific steps:
preparing a molybdenum disulfide precursor;
dissolving sodium molybdate dihydrate and thiourea in polyethylene glycol-400, stirring uniformly, transferring the obtained solution into a three-neck bottle, and performing microwave treatment for a period of time at a certain temperature and under a certain power to obtain a molybdenum disulfide precursor.
The mass ratio of the sodium molybdate dihydrate to the thiourea is 1: 1.2-1: 2.6; the concentration of the sodium molybdate dihydrate in the polyethylene glycol-400 is 8.3 mg/mL-10 mg/mL.
The reaction temperature is 160-180 ℃; the microwave processing power is 600W-900W; the microwave treatment time is 3-10 min.
Step two, high-temperature heat treatment;
and washing the obtained molybdenum disulfide precursor with water and ethanol for more than 2 times to remove impurities, and then carrying out vacuum drying. The dried sample is then calcined under an inert atmosphere at a temperature and for a period of time.
The vacuum drying temperature is 60-80 ℃;
the high-temperature calcination temperature is 600-800 ℃; the calcination temperature is 1-2 hours.
Step three, preparing the anode of the aluminum ion battery;
weighing a certain amount of the obtained molybdenum disulfide material, mixing the molybdenum disulfide material with conductive carbon black and a binding agent polyvinylidene fluoride according to a mass ratio of 8:1:1, fully grinding, dripping a proper amount of N-methyl-2-pyrrolidone by using a dropper, fully stirring, coating the uniformly mixed electrode material on tantalum foil, and drying for 8-12 hours at 60-80 ℃ by using a vacuum drying oven. Then, a 2032 type button cell was assembled by using a metal aluminum counter electrode and a glass fiber membrane (GF/D) as separators and an ionic liquid as an electrolyte, the ionic liquid being prepared from anhydrous aluminum chloride and 1-ethyl-3-methylimidazolium chloride in a molar ratio of 1.3: 1. And then, carrying out electrochemical performance test on the prepared battery at a voltage range of 0.01-2.0V by using a LAND-CT2001A battery test system.
The test result shows that the molybdenum disulfide material obtained by the invention has good cycling stability, and the discharge capacity is still well maintained even at high current density. When 100mA g is selected-1The current density is taken as the test current, and after 100 cycles of charge and discharge, the specific capacity of the electrode material still reaches 48.1mAh g-1。
The molybdenum disulfide material obtained by the invention is characterized in that: the spherical molybdenum disulfide has a spherical structure with the grain diameter of about 200 nanometers formed by piling flaky molybdenum disulfide with small grain diameter, and has larger specific surface area and good structural stability.
Compared with the prior art, the invention has the beneficial effects that:
(1) the raw materials adopted by the invention are sodium molybdate dihydrate and thiourea, the material source is simple, the green and safe effects are realized, the price is low, and the large-scale production can be realized.
(2) By adopting a microwave treatment method, the obtained monolithic flaky molybdenum disulfide is orderly stacked into a spherical material, and the structural stability of the material is good.
(3) The electrode material obtained by the method has high specific capacity, and the capacity of the electrode material is well maintained.
Drawings
FIG. 1 shows scanning electron microscope and projection electron microscope photographs of molybdenum disulfide material, which are processed by microwave at 800W power for 3min and constant temperature at 800 deg.C for 2 hours.
FIG. 2 is an XRD picture of molybdenum disulfide material, which is treated with microwave at 800W power for 3min and then treated at 800 deg.C for 2 hours.
FIG. 3 shows that the molybdenum disulfide material obtained by microwave treatment with 800W power for 3min and constant temperature treatment at 800 ℃ for 2 hours is 100mA g-1Current density of (a).
FIG. 4 shows that the molybdenum disulfide material obtained by microwave treatment with 700W power for 3min and heat treatment at 800 deg.C is 100mA g-1Current density of (a).
FIG. 5 shows disulfide obtained by microwave treatment at 800W power for 6min and constant temperature treatment at 800 deg.CMolybdenum material at 100mA g-1Current density of (a).
FIG. 6 shows that the power of 800W is microwave treated for 3min, the constant temperature treatment at 800 ℃ and the molybdenum disulfide material prepared by the solution heat method is at 100mA g-1Current density of (a).
Detailed Description
The invention will be described in further detail below with reference to the drawings and examples.
The invention relates to a preparation method of a molybdenum disulfide aluminum ion battery electrode material, which comprises the following steps:
preparing a molybdenum disulfide precursor;
dissolving sodium molybdate dihydrate and thiourea in polyethylene glycol-400, stirring uniformly, transferring the obtained solution into a three-neck bottle, and performing microwave treatment for a period of time at a certain temperature and under a certain power to obtain a molybdenum disulfide precursor.
The mass ratio of the sodium molybdate dihydrate to the thiourea is 1: 1.2-1: 2.6; the concentration of the sodium molybdate dihydrate in the polyethylene glycol-400 is 8.3 mg/mL-10 mg/mL.
The reaction temperature is 160-180 ℃; the microwave processing power is 600W-900W; the microwave treatment time is 3-10 Min.
Step two, high-temperature heat treatment;
and washing the obtained molybdenum disulfide precursor with water and ethanol for more than 2 times to remove impurities, and then carrying out vacuum drying. The dried sample is then calcined under an inert atmosphere at a temperature and for a period of time.
The vacuum drying temperature is 60-80 ℃;
the high-temperature calcination temperature is 600-800 ℃; the calcination temperature is 1-2 hours.
Step three, preparing the anode of the aluminum ion battery;
weighing a certain amount of the obtained molybdenum disulfide material, mixing the molybdenum disulfide material with conductive carbon black and a binding agent polyvinylidene fluoride according to a mass ratio of 8:1:1, fully grinding, dripping a proper amount of N-methyl-2-pyrrolidone by using a dropper, fully stirring, coating the uniformly mixed electrode material on tantalum foil, and drying for 8-12 hours at 60-80 ℃ by using a vacuum drying oven. Then, a 2032 type button cell was assembled by using a metal aluminum counter electrode and a glass fiber membrane (GF/D) as separators and an ionic liquid as an electrolyte, the ionic liquid being prepared from anhydrous aluminum chloride and 1-ethyl-3-methylimidazolium chloride in a molar ratio of 1.3: 1. And then, carrying out electrochemical performance test on the prepared battery at a voltage range of 0.01-2.0V by using a LAND-CT2001A battery test system.
Example 1
Preparing a molybdenum disulfide precursor;
weighing 0.35g of sodium molybdate dihydrate and 0.45g of thiourea, mixing and dissolving in 50mL of polyethylene glycol-400, stirring uniformly, transferring the obtained solution into a 300mL three-necked bottle, and treating for 3Min at 160 ℃ and 800W to obtain a molybdenum disulfide precursor;
step two, high-temperature heat treatment;
and respectively washing the obtained molybdenum disulfide precursor with deionized water and ethanol for 3 times to remove impurities, and then drying in a vacuum oven at 70 ℃. The dried sample was then calcined at 800 ℃ for 2 hours under argon atmosphere.
Step three, preparing the anode of the aluminum ion battery;
weighing 80mg of the obtained molybdenum disulfide material, mixing the molybdenum disulfide material with conductive carbon black and a binding agent polyvinylidene fluoride according to the mass ratio of 8:1:1, fully grinding, dripping 3 drops of N-methyl-2-pyrrolidone by a dropper, fully stirring, coating the uniformly mixed electrode material on tantalum foil, and drying for 12 hours at 80 ℃ by using a vacuum drying oven. Then, a 2032 type button cell was assembled by using a metal aluminum counter electrode and a glass fiber membrane (GF/D) as separators and an ionic liquid as an electrolyte, the ionic liquid being prepared from anhydrous aluminum chloride and 1-ethyl-3-methylimidazolium chloride in a molar ratio of 1.3: 1. And then, carrying out electrochemical performance test on the prepared battery at a voltage range of 0.01-2.0V by using a LAND-CT2001A battery test system.
Fig. 1(a) is an environmental scan of the molybdenum disulfide material, and it can be seen that the material has a sheet structure and relatively uniform size. From the transmission electron micrograph of fig. 1(b), it can be seen that the nanosheets have a particle size of about 10 nm and have a monolayer or bilayer structure.
Fig. 2 is an XRD picture of the obtained molybdenum disulfide material. The figure shows that the sample has typical characteristic peaks (022), (100), (103), (110), (201) and the like of molybdenum disulfide, and the synthesized sample is proved to be molybdenum disulfide.
FIG. 3 shows the current at 100mA g-1Discharge curve of the prepared material at the current density of (2). It is obvious from the figure that the prepared molybdenum disulfide material has good cycling stability, and the specific discharge capacity of the molybdenum disulfide material can still be kept at 48.1mAh g after 100 times of charge-discharge cycles-1。
Example 2
Preparing a molybdenum disulfide precursor;
weighing 0.5g of sodium molybdate dihydrate and 0.65g of thiourea, mixing and dissolving in 60mL of polyethylene glycol-400, stirring uniformly, transferring the obtained solution into a 300mL three-neck bottle, and processing for 3Min at 160 ℃ and 700W to obtain a molybdenum disulfide precursor;
step two, high-temperature heat treatment;
the obtained molybdenum disulfide precursor was washed with deionized water and ethanol 3 times, respectively, to remove impurities, and then dried in a vacuum oven at 70 ℃. The dried sample was then calcined at 800 ℃ for 2 hours under argon atmosphere.
Step three, preparing the anode of the aluminum ion battery;
weighing 100mg of the obtained molybdenum disulfide material, mixing the molybdenum disulfide material with conductive carbon black and a binding agent polyvinylidene fluoride according to a mass ratio of 8:1:1, fully grinding, dripping 5 drops of N-methyl-2-pyrrolidone by a dropper, fully stirring, coating the uniformly mixed electrode material on tantalum foil, and drying for 12 hours at 80 ℃ by using a vacuum drying oven. Then, a 2032 type button cell was assembled by using a metal aluminum counter electrode and a glass fiber membrane (GF/D) as separators and an ionic liquid as an electrolyte, the ionic liquid being prepared from anhydrous aluminum chloride and 1-ethyl-3-methylimidazolium chloride in a molar ratio of 1.3: 1. And then, carrying out electrochemical performance test on the prepared battery at a voltage range of 0.01-2.0V by using a LAND-CT2001A battery test system.
The process of the present invention was substantially the same as that employed in example 1 except that the microwave treatment power was 700W. The electrode material was mixed with the material prepared in example 1 at 100mA g-1The discharge curve at the current density of (a) is shown in fig. 4, from which it can be seen that the specific discharge capacity of the material prepared by the method used in this example is lower than that of example 1 at the same current density. The reason is that the microwave treatment power influences the size and shape of the synthesized molybdenum disulfide, and further influences the electrochemical performance of the synthesized molybdenum disulfide. By contrast, 800W is found to be a better microwave processing power.
Example 3
Preparing a molybdenum disulfide precursor;
weighing 0.30g of sodium molybdate dihydrate and 0.40g of thiourea, mixing and dissolving in 30mL of polyethylene glycol-400, stirring uniformly, transferring the obtained solution into a 300mL three-neck bottle, and treating for 6Min at 160 ℃ and 800W to obtain a molybdenum disulfide precursor;
step two, high-temperature heat treatment;
the obtained molybdenum disulfide precursor was washed with deionized water and ethanol 3 times, respectively, to remove impurities, and then dried in a vacuum oven at 70 ℃. The dried sample was then calcined at 800 ℃ for 2 hours under argon atmosphere.
Step three, preparing the anode of the aluminum ion battery;
weighing 80mg of the obtained molybdenum disulfide material, mixing the molybdenum disulfide material with conductive carbon black and a binding agent polyvinylidene fluoride according to the mass ratio of 8:1:1, fully grinding, dripping 3 drops of N-methyl-2-pyrrolidone by a dropper, fully stirring, coating the uniformly mixed electrode material on tantalum foil, and drying for 12 hours at 80 ℃ by using a vacuum drying oven. Then, a 2032 type button cell was assembled by using a metal aluminum counter electrode and a glass fiber membrane (GF/D) as separators and an ionic liquid as an electrolyte, the ionic liquid being prepared from anhydrous aluminum chloride and 1-ethyl-3-methylimidazolium chloride in a molar ratio of 1.3: 1. And then, carrying out electrochemical performance test on the prepared battery at a voltage range of 0.01-2.0V by using a LAND-CT2001A battery test system.
The invention is essentially the same as the method used in example 1, except that the microwave treatment time is changed to 6 Min. The electrode material was mixed with the material prepared in example 1 at 100mA g-1The discharge curve at the current density of (a) is shown in fig. 5, from which it can be seen that the specific discharge capacity of the material prepared by the method used in this example is lower than that of example 1 at the same current density. This is because the microwave treatment time affects the size and morphology of the synthesized molybdenum disulfide. By comparison, 3Min is a better microwave treatment time.
Comparative example 1
Preparing a molybdenum disulfide precursor;
weighing 0.35g of sodium molybdate dihydrate and 0.45g of thiourea, mixing and dissolving in 50mL of polyethylene glycol-400, stirring uniformly, transferring the obtained solution into a 100mL reaction kettle with polytetrafluoroethylene as a lining, and preserving heat at 180 ℃ for 20 hours to obtain a molybdenum disulfide precursor;
step two, high-temperature heat treatment;
and respectively washing the obtained molybdenum disulfide precursor with deionized water and ethanol for 3 times to remove impurities, and then drying in a vacuum oven at 70 ℃. The dried sample was then calcined at 800 ℃ for 2 hours under argon atmosphere.
Step three, preparing the anode of the aluminum ion battery;
weighing 80mg of the obtained molybdenum disulfide material, mixing the molybdenum disulfide material with conductive carbon black and a binding agent polyvinylidene fluoride according to the mass ratio of 8:1:1, fully grinding, dripping 3 drops of N-methyl-2-pyrrolidone by a dropper, fully stirring, coating the uniformly mixed electrode material on tantalum foil, and drying for 12 hours at 80 ℃ by using a vacuum drying oven. Then, a 2032 type button cell was assembled by using a metal aluminum counter electrode and a glass fiber membrane (GF/D) as separators and an ionic liquid as an electrolyte, the ionic liquid being prepared from anhydrous aluminum chloride and 1-ethyl-3-methylimidazolium chloride in a molar ratio of 1.3: 1. And then, carrying out electrochemical performance test on the prepared battery at a voltage range of 0.01-2.0V by using a LAND-CT2001A battery test system.
The invention and that adopted in example 1The method is basically the same, except that the reaction mode is changed into solvothermal, and the heating time is prolonged by 400 times. The electrode material was mixed with the material prepared in example 1 at 100mA g-1The discharge curve at the current density of (a) is shown in fig. 6, and it can be seen from the graph that the specific discharge capacity of the material prepared by the method of the present comparative example is much lower than that of example 1 at the same current density. This is because the microwave treatment affects the size and morphology of the synthesized molybdenum disulfide. By comparison, the molybdenum sulfide obtained by microwave treatment has better performance than that of the molybdenum sulfide generated by solvothermal reaction and used as the anode material of the aluminum ion battery.
Comparative example 2
Preparing a molybdenum disulfide precursor;
weighing 0.35g of sodium molybdate dihydrate and 0.45g of thiourea, mixing and dissolving in 50mL of deionized water, stirring until the solution is uniform, transferring the obtained solution into a 300mL three-necked bottle, and processing for 3Min at the temperature of 100 ℃ and the power of 800W to obtain a molybdenum disulfide precursor;
step two, high-temperature heat treatment;
and respectively washing the obtained molybdenum disulfide precursor with deionized water and ethanol for 3 times to remove impurities, and then drying in a vacuum oven at 70 ℃. The dried sample was then calcined at 800 ℃ for 2 hours under argon atmosphere.
Step three, preparing the anode of the aluminum ion battery;
weighing 80mg of the obtained molybdenum disulfide material, mixing the molybdenum disulfide material with conductive carbon black and a binding agent polyvinylidene fluoride according to the mass ratio of 8:1:1, fully grinding, dripping 3 drops of N-methyl-2-pyrrolidone by a dropper, fully stirring, coating the uniformly mixed electrode material on tantalum foil, and drying for 12 hours at 80 ℃ by using a vacuum drying oven. Then, a 2032 type button cell was assembled by using a metal aluminum counter electrode and a glass fiber membrane (GF/D) as separators and an ionic liquid as an electrolyte, the ionic liquid being prepared from anhydrous aluminum chloride and 1-ethyl-3-methylimidazolium chloride in a molar ratio of 1.3: 1. And then, carrying out electrochemical performance test on the prepared battery at a voltage range of 0.01-2.0V by using a LAND-CT2001A battery test system.
The process of the present invention was substantially the same as that used in example 1 except that the solvent used was deionized water. The specific discharge capacity of the material prepared by the method of the comparative example is much lower than that of the material prepared by the example 1 under the same current density. The reason is that the boiling point of water as a reaction solvent is 100 ℃, and the low temperature can influence the size, the shape and the yield of the synthesized molybdenum disulfide. By comparison, the molybdenum disulfide material generated by using the polyethylene glycol-400 as a reaction solvent has better performance as the anode of the aluminum ion battery.
Claims (6)
1. A molybdenum sulfide material characterized by: the spherical molybdenum disulfide is stacked into a spherical structure with the particle size of 180-200 nanometers by using flaky molybdenum disulfide with the thickness of 1-2 nanometers.
2. The molybdenum sulfide material of claim 1, wherein: the interval between two farthest points on the side edge of the lamellar surface of the flaky molybdenum disulfide is 5-15 nanometers or the diameter of the lamellar surface of the flaky molybdenum disulfide is 5-15 nanometers.
3. A method of producing a molybdenum sulfide material according to claim 1 or 2, wherein:
1) preparing a molybdenum disulfide precursor;
dissolving sodium molybdate dihydrate and thiourea in polyethylene glycol-400, stirring uniformly, transferring the obtained solution into a container, and performing microwave treatment for a period of time at a certain reaction temperature and under a certain power to obtain a molybdenum disulfide precursor;
the mass ratio of the sodium molybdate dihydrate to the thiourea is 1: 1.2-1: 2.6; the concentration of the sodium molybdate dihydrate in the polyethylene glycol-400 is 8.3 mg/mL-10 mg/mL;
the reaction temperature is 160-180 ℃; the microwave processing power is 600W-900W; the microwave treatment time is 3-10 min;
2) high-temperature heat treatment;
washing the molybdenum disulfide precursor with water and ethanol for more than 2 times in sequence to remove impurities, and then drying in vacuum; then calcining the sample at a certain temperature for a period of time under an inert atmosphere;
the vacuum drying temperature is 60-80 ℃;
the high-temperature calcination temperature is 600-800 ℃; the calcination temperature is 1-2 hours.
4. The method of claim 3, wherein: the inert atmosphere is nitrogen and/or argon.
5. Use of the molybdenum sulfide material of claim 1 or 2 as a positive electrode active material in an aluminum ion battery positive electrode.
6. Use according to claim 5, characterized in that:
the positive electrode material of the aluminum ion battery comprises the following components in a mass ratio of 8:1:1, conductive carbon black and a binder polyvinylidene fluoride.
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| CN112079385A (en) * | 2020-08-11 | 2020-12-15 | 扬州大学 | Aluminum ion battery positive electrode material and preparation method thereof |
| CN113247954A (en) * | 2021-05-12 | 2021-08-13 | 中山大学 | Large-interlayer-distance molybdenum disulfide material and preparation method and application thereof |
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| CN107188231A (en) * | 2017-06-21 | 2017-09-22 | 淮北师范大学 | A kind of preparation method of the micro-nano hierarchy of the spherical molybdenum disulfide of high dispersive |
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| CN112079385A (en) * | 2020-08-11 | 2020-12-15 | 扬州大学 | Aluminum ion battery positive electrode material and preparation method thereof |
| CN113247954A (en) * | 2021-05-12 | 2021-08-13 | 中山大学 | Large-interlayer-distance molybdenum disulfide material and preparation method and application thereof |
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