CN108054359B - Preparation method of molybdenum disulfide intercalation material - Google Patents

Preparation method of molybdenum disulfide intercalation material Download PDF

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CN108054359B
CN108054359B CN201711286874.8A CN201711286874A CN108054359B CN 108054359 B CN108054359 B CN 108054359B CN 201711286874 A CN201711286874 A CN 201711286874A CN 108054359 B CN108054359 B CN 108054359B
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molybdenum disulfide
intercalation
intercalation material
sodium molybdate
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杨金虎
冯楠
黄继梅
祖连海
刘光磊
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Tongji University
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    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01MPROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
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    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01MPROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00Electrodes
    • H01M4/02Electrodes composed of, or comprising, active material
    • H01M4/36Selection of substances as active materials, active masses, active liquids
    • H01M4/58Selection of substances as active materials, active masses, active liquids of inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy; of polyanionic structures, e.g. phosphates, silicates or borates
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Abstract

The invention relates to a preparation method of a molybdenum disulfide intercalation material, which comprises the following steps of (1) mixing sodium molybdate and thioacetamide, and adding a solvent for dissolving; (2) heating the mixed solution in the step (1) to perform a solvothermal reaction; (3) cooling the product obtained in the step (2) and then centrifuging and washing; (4) taking linear macromolecules to carry out ultrasonic uniform mixing intercalation on the product obtained in the step (3), and then transferring the product to a freeze dryer for freeze drying; (5) and (4) placing the sample in the step (4) into a tubular furnace for calcination to prepare the molybdenum disulfide intercalation material. According to the molybdenum disulfide/carbon heterojunction material prepared by the invention, the carbon chains are supported between layers and between sheets, so that not only are interlayer active sites provided, but also a quick channel is provided for ion transmission between sheets, and simultaneously, the conductivity of molybdenum disulfide is greatly improved, so that each sheet layer can effectively store energy.

Description

Preparation method of molybdenum disulfide intercalation material
Technical Field
The invention relates to the field of energy storage devices, in particular to a preparation method of a molybdenum disulfide intercalation material.
Background
The chemical power source is a device capable of realizing mutual conversion of electric energy and chemical energy, and is an important medium capable of more reasonably utilizing energy. Chemical power sources, represented by lithium ion batteries and supercapacitors, have extremely wide applications. The lithium ion battery has the excellent performances of high working voltage, high energy density, low self-discharge rate, long cycle life, no memory effect and the like, and also has the defects of low power density, poor cycle stability and the like; the super capacitor has a plurality of excellent performances of high charging speed, long cycle service life, high energy conversion efficiency, high safety factor and the like, but the problem of low power density and the like are still difficult to solve. With the further development of the new generation of energy storage devices, the development of electrode materials with more excellent performance becomes a problem to be solved urgently. Molybdenum disulfide is a typical transition metal binary compound and has a graphene-like structure. And a covalent bond is formed between Mo and S atoms in the layer, so that the structure is very stable. Molybdenum disulfide has unique physicochemical properties, has been widely used for electrochemical energy storage, and exhibits excellent performance. The research core of the current molybdenum disulfide material is to carry out the effective intercalation of 002 crystal face. Specifically, in the field of super capacitors, the conduction rate of electrons and ions is improved by introducing a high-conductivity carbon material into an interlayer 002 crystal face, so that active sites in the layer are fully utilized, and high-power and high-energy storage is realized.
Chinese patent CN106848228A discloses a method for preparing a molybdenum disulfide/carbon composite hierarchical pore material, which comprises the steps of adding water to sodium molybdate, thioacetamide and agarose for dissolution, heating in a water bath, pouring out and cooling when the reaction is finished, transferring the cooled sample to a refrigerator for freezing, transferring to a freeze dryer for drying, and finally placing in a tubular furnace for calcining to obtain the molybdenum disulfide/carbon composite hierarchical pore material. Although macroscopically the same aerogel material, the patent can only refer to a simple composite structure of carbon material and molybdenum disulfide, and cannot refer to a heterojunction structure at a nanometer scale, and the aerogel material is mainly a carbon skeleton formed by agarose.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provide a preparation method of a molybdenum disulfide intercalation material.
The purpose of the invention can be realized by the following technical scheme:
a preparation method of a molybdenum disulfide intercalation material comprises the following steps:
(1) mixing sodium molybdate and thioacetamide, and adding a solvent for dissolving;
(2) heating the mixed solution in the step (1) to perform a solvothermal reaction;
(3) cooling the product obtained in the step (2) and then centrifuging and washing;
(4) taking linear macromolecules to carry out ultrasonic uniform mixing intercalation on the product obtained in the step (3), and then transferring the product to a freeze dryer for freeze drying;
(5) and (4) placing the sample in the step (4) into a tubular furnace for calcination to prepare the molybdenum disulfide intercalation material.
The mass ratio of the sodium molybdate to the thioacetamide in the step (1) is 0.3-0.6: 0.6-1.2, and the solvent is a mixed solvent obtained by mixing water and ethylene glycol according to the volume ratio of 2: 1. The concentration of the sodium molybdate in the solvent is controlled to be 0.01-0.02 g/ml.
The temperature of the solvothermal reaction in the step (2) is 200-240 ℃, and the reaction time is 20-24 h.
And (4) in the step (3), the centrifugal washing is carried out by alternately washing three times by adopting water and ethanol.
The linear polymer in the step (4) comprises polyethyleneimine or polyethylene glycol, and the mass of the linear polymer is 20% -100% of that of the molybdenum disulfide molecules. The ultrasonic frequency of the ultrasonic mixing intercalation is 360-440HZ, and the time is 1-3 h. The freeze drying temperature is controlled to be 56-40 ℃ below zero, and the time is 12-24 hours.
The calcination in the step (5) is controlled at the temperature of 600 ℃ and 800 ℃ for 2-6 hours, and the heating rate is 2-5 ℃ per minute.
This application utilizes the polymer to realize effective intercalation to molybdenum disulfide, make original intrinsic 0.62 nm's interlamellar spacing of molybdenum disulfide enlarge to 0.95nm on the nanometer scale, the support of carbon chain between layer and piece, not only provide the active site between the layer, and for piece ion transmission provides swift passageway, molybdenum disulfide's electric conductivity has still been improved greatly simultaneously, make every lamella can both effectively store energy, be arranged in the ultracapacitor system have specific capacity height, the cycle performance is good, characteristics such as stable in structure, be an excellent energy storage material, use molybdenum disulfide as major structure.
The present application benefits from material selection in the first place. Molybdenum disulfide is a two-dimensional material with a layered graphene-like structure, and the layers of the molybdenum disulfide are supported by weak van der waals force; the surface of the molybdenum disulfide material synthesized by the hydrothermal method is provided with negative charges, and the high-molecular polyethyleneimine is provided with positive charges, so that the electrostatic acting force of the positive charges and the negative charges which are mutually attracted plays a very large role in intercalation driving force; in addition, in molecular dynamics, the ultrasonic boosting with the frequency of 400Hz is beneficial to accelerating the movement and uniform mixing of two molecules.
Compared with the prior art, the molybdenum disulfide/carbon heterojunction material is prepared by the method, the carbon chain is inserted between the molybdenum disulfide layers, the active sites between the layers are improved, meanwhile, a good supporting effect is also achieved between the sheets, the agglomeration of the molybdenum disulfide sheets is effectively prevented, and a quick channel is provided for ion transmission. Meanwhile, the conductivity of the molybdenum disulfide is greatly improved, each lamella can effectively store energy, and the molybdenum disulfide super capacitor has the advantages of high specific capacity, good cycle performance, stable structure and the like and is an excellent energy storage material.
Drawings
FIG. 1 is a scanning electron micrograph of molybdenum disulfide intercalated materials prepared in examples 1, 2, 3 and 4.
Figure 2 is a transmission electron micrograph of the molybdenum disulfide intercalation material prepared in example 1.
FIG. 3 is an XRD and Raman diagram of the molybdenum disulfide intercalation material prepared in example 1.
Figure 4 is a plot of the charge and discharge performance of a supercapacitor assembled with a molybdenum disulfide intercalation material prepared in example 1.
Detailed Description
The present invention will be described in detail with reference to specific examples. The following examples will assist those skilled in the art in further understanding the invention, but are not intended to limit the invention in any way. It should be noted that variations and modifications can be made by persons skilled in the art without departing from the spirit of the invention. All falling within the scope of the present invention.
Example 1
0.3 g of sodium molybdate and 0.6 g of thioacetamide were added to the reaction vessel and dissolved by adding 20 ml of water and 10 ml of ethylene glycol. And (3) putting the reaction kettle into an oven, heating to perform solvothermal reaction, and setting the temperature of the oven to be 220 ℃. After 24 hours of reaction, the device is closed, and after cooling, molybdenum disulfide is obtained by centrifugal washing. And then, taking linear high molecular polyethyleneimine with the molecular weight of 600 to carry out ultrasonic uniform mixing intercalation on the molybdenum disulfide sample, and then transferring the molybdenum disulfide sample to a freeze dryer with the temperature of-56 ℃ for drying for 24 hours. The sample was calcined in a tube furnace at 800 ℃ for 6 hours at a rate of 2 ℃ per minute. The prepared sample is shown in fig. 1A, which can show that the molybdenum disulfide synthesized by the hydrothermal method is uniformly distributed in a flower-sheet shape, has no obvious accumulation and agglomeration, and presents a certain transparency, which indicates that the molybdenum disulfide has very thin sheet layers and contains a small amount of uniformly distributed partially graphitized carbon between layers and between sheets.
Figure 2 is a transmission electron micrograph of the molybdenum disulfide intercalation material prepared in example 1. FIGS. A and B show the MoS2The low-power transmission picture of the/C heterojunction aerogel material is characterized in that a molybdenum disulfide layer is in a certain bent folding shape along with the intercalation of high molecules, and the existence of partially crystallized graphite carbon can be obviously seen between the layers and the sheets of the molybdenum disulfide; panel C is a further measure of the expansion of the heterojunction material after intercalation from the original 0.62nm to 0.95 nm. And the intercalation of carbon has certain disturbance effect on the arrangement of molybdenum disulfide atoms in the surface, so that the arrangement of in-plane lattices is twisted to a certain degree, as shown in figure D. FIG. 3 is an XRD and Raman diagram of the molybdenum disulfide intercalation material prepared in example 1. Analyzing the crystal structure of the sample by adopting X-ray diffraction and Raman spectroscopy to find the h-MoS as the raw material before intercalation2The diffraction peak positions of (c) are mainly at the positions of 13.8 °, 33.1 °, 40.3 ° and 60.0 °, as shown in fig. 3A, corresponding to the (002), (100), (103), and (100) crystal planes (JCPDS card 37-1492), respectively. No matter the PEI or PEG is a macromolecule, the 002 peak position after intercalation is obviously moved forward, and each of 8.9 degrees and 17.6 degrees is provided with an obvious peak which is respectively marked as a peak 1 and a peak 2, the corresponding interlayer spacing is 0.98nm, and is enlarged by nearly 0.33nm compared with the 002 surface spacing of pure molybdenum disulfide by 0.65nm, and the distance is just corresponding to a layer of carbon. This is due to the fact that the macromolecule is effectively inserted between the layers of the molybdenum disulfide molecule, and the high-temperature heat is processed under the inert protective atmosphereAfter treatment, the carbon that the polymer became partially graphitized remained between the layers, and the experimental results were consistent with the data observed by TEM. FIG. 3B shows the results of Raman spectroscopy on h-MoS21gAnd E2gPeaks of vibration modes were located at 375.6 and 405.9cm, respectively-1Out-of-plane vibration and in-plane vibration of the Mo-S bond are represented, respectively. For the intercalated material, whether PEG or PEI, the heterojunction material after intercalation is 1350.1 and 1590.9cm-1Both have two strong peaks corresponding to the D and G peaks of the intercalated carbon material. And the intercalation of the macromolecule has certain interference on the vibration frequency of the molybdenum disulfide per se, so that A1gAnd E2gHas certain red shift and blue shift, and the shifted peak positions are 378.1 cm and 403.2cm respectively-1. Figure 4 is a plot of the charge and discharge performance of a supercapacitor assembled with a molybdenum disulfide intercalation material prepared in example 1. In 1Ag-1At times, the capacity is as high as 4143.8F g-1. The heterojunction electrode material with expanded interlayer spacing is obtained by calcining the high polymer material due to effective intercalation. The intercalation of carbon chain between molybdenum disulfide layer and support between the piece have not only improved the active site between the layer, have provided swift passageway for the ionic transmission between the piece moreover, have still improved molybdenum disulfide's electric conductivity greatly simultaneously for every lamella can both effectively store energy, consequently has obtained super high energy storage effect, and at high magnification 10Ag-1The capacity can reach 2483.02F g-1
Example 2
0.3 g of sodium molybdate and 0.6 g of thioacetamide were added to the reaction vessel and dissolved by adding 20 ml of water and 10 ml of ethylene glycol. And (3) putting the reaction kettle into an oven, heating to perform solvothermal reaction, and setting the temperature of the oven to be 220 ℃. After 24 hours of reaction, the device is closed, and after cooling, molybdenum disulfide is obtained by centrifugal washing. And then, taking linear high molecular polyethyleneimine with the molecular weight of 70000 to carry out ultrasonic uniform mixing intercalation on the molybdenum disulfide sample, and then transferring the molybdenum disulfide sample to a freeze dryer with the temperature of minus 56 ℃ for drying for 24 hours. The sample was calcined in a tube furnace at 800 ℃ for 6 hours at a rate of 2 ℃ per minute. The prepared sample is shown in fig. 1B, which can show that the molybdenum disulfide synthesized by the hydrothermal method is uniformly distributed in a flower-sheet shape, has no obvious accumulation and agglomeration, and presents a certain transparency, indicating that the molybdenum disulfide has very thin sheet layers, and contains a small amount of uniformly distributed partially graphitized carbon between layers and between sheets. The figure also shows that for the same type of polymer, different molecular weight intercalation has little influence on the appearance of the sample, and the intercalation capability of the polymer PEI is stronger.
Example 3
0.3 g of sodium molybdate and 0.6 g of thioacetamide were added to the reaction vessel and dissolved by adding 20 ml of water and 10 ml of ethylene glycol. And (3) putting the reaction kettle into an oven, heating to perform solvothermal reaction, and setting the temperature of the oven to be 220 ℃. After 24 hours of reaction, the device is closed, and after cooling, molybdenum disulfide is obtained by centrifugal washing. And then, taking linear high molecular polyethylene glycol with the molecular weight of 400 to carry out ultrasonic uniform mixing intercalation on the molybdenum disulfide sample, and then transferring the molybdenum disulfide sample to a freeze dryer with the temperature of minus 56 ℃ for drying for 24 hours. The sample was calcined in a tube furnace at 800 ℃ for 6 hours at a rate of 2 ℃ per minute. The prepared sample is shown in fig. 1C, which shows that the molybdenum disulfide synthesized by the hydrothermal method is uniformly distributed in a flower-sheet shape, has no obvious accumulation and agglomeration, and presents a certain transparency, indicating that the molybdenum disulfide has very thin sheet layers, and contains a small amount of uniformly distributed partially graphitized carbon between layers and between sheets. The figure also shows that different polymers with similar molecular weights have the same intercalation effect and similar appearance.
Example 4
0.3 g of sodium molybdate and 0.6 g of thioacetamide were added to the reaction vessel and dissolved by adding 20 ml of water and 10 ml of ethylene glycol. And (3) putting the reaction kettle into an oven, heating to perform solvothermal reaction, and setting the temperature of the oven to be 220 ℃. After 24 hours of reaction, the device is closed, and after cooling, molybdenum disulfide is obtained by centrifugal washing. And then, taking linear macromolecular polyethylene glycol with the molecular weight of 20000 to carry out ultrasonic uniform mixing intercalation on the molybdenum disulfide sample, and then transferring the molybdenum disulfide sample to a freeze dryer with the temperature of minus 56 ℃ for drying for 24 hours. The sample was calcined in a tube furnace at 800 ℃ for 6 hours at a rate of 2 ℃ per minute. The prepared sample is shown in fig. 1D, which can show that the molybdenum disulfide synthesized by the hydrothermal method is uniformly distributed in a flower-like sheet shape, has no obvious accumulation and agglomeration, and presents a certain transparency, indicating that the molybdenum disulfide sheet layer is very thin, and contains a small amount of uniformly distributed partially graphitized carbon between layers and between sheets, and the figure simultaneously shows that for the same type of polymer, different molecular weight intercalation layers have little influence on the sample morphology.
Compared with the prior art, the molybdenum disulfide special intercalation structural material synthesized by the method realizes effective intercalation of molybdenum disulfide molecules by high molecules for the first time, and the high-molecular materials with different types and different molecular weights can be selected to prepare the M-C-M sandwich heterojunction electrode material with enlarged interlayer spacing, so that the electrode material has good conductivity, simple preparation method and strong innovation. The support of carbon chain between layer and piece not only provides the active site between the layer, provides swift passageway for inter-piece ion transmission moreover, has still improved molybdenum disulfide's electric conductivity simultaneously greatly for every lamella can both effectively store energy, has advantages such as specific capacity height, good, the stable in structure of cycling performance for among the ultracapacitor system.
Example 5
A preparation method of a molybdenum disulfide intercalation material comprises the following steps:
(1) mixing sodium molybdate and thioacetamide, adding water and glycol in a volume ratio of 2:1 to obtain a mixed solvent, dissolving, wherein the mass ratio of the sodium molybdate to the thioacetamide is 0.3:1.2, and controlling the concentration of the sodium molybdate in the solvent to be 0.01 g/ml;
(2) heating the mixed solution in the step (1) to 200 ℃ to carry out solvothermal reaction for 24 h;
(3) cooling the product obtained in the step (2), and then alternately centrifuging and washing the product by using water and ethanol for three times;
(4) carrying out ultrasonic blending and intercalation on the product obtained in the step (3) by using polyethyleneimine, wherein the added mass of the polyethyleneimine is 20% of that of molybdenum disulfide, the ultrasonic frequency is controlled to be 360HZ during ultrasonic treatment, the time is 3h, then transferring the product to a freeze dryer, the temperature is controlled to be minus 56 ℃, and freeze drying is carried out for 12 hours;
(5) and (4) placing the sample in the step (4) into a tube furnace, controlling the heating rate to be 2 ℃ per minute, and heating to 600 ℃ for 6 hours to prepare the molybdenum disulfide intercalation material.
Example 6
A preparation method of a molybdenum disulfide intercalation material comprises the following steps:
(1) mixing sodium molybdate and thioacetamide, adding water and glycol in a volume ratio of 2:1 to obtain a mixed solvent, dissolving, wherein the mass ratio of the sodium molybdate to the thioacetamide is 0.4:0.9, and controlling the concentration of the sodium molybdate in the solvent to be 0.01 g/ml;
(2) heating the mixed solution in the step (1) to 220 ℃ to carry out solvothermal reaction for 24 h;
(3) cooling the product obtained in the step (2), and then alternately centrifuging and washing the product by using water and ethanol for three times;
(4) carrying out ultrasonic blending and intercalation on the product obtained in the step (3) by using polyethyleneimine, wherein the added mass of the polyethyleneimine is 50% of that of molybdenum disulfide, the ultrasonic frequency is controlled to be 400HZ during ultrasonic treatment, the time is 2 hours, then transferring the product to a freeze dryer, the temperature is controlled to be 50 ℃ below zero, and freeze drying is carried out for 18 hours;
(5) and (4) placing the sample in the step (4) into a tube furnace, controlling the heating rate to be 3 ℃ per minute, and heating to 700 ℃ for 5 hours to prepare the molybdenum disulfide intercalation material.
Example 7
A preparation method of a molybdenum disulfide intercalation material comprises the following steps:
(1) mixing sodium molybdate and thioacetamide, adding water and glycol in a volume ratio of 2:1 to obtain a mixed solvent, dissolving, wherein the mass ratio of the sodium molybdate to the thioacetamide is 0.6:0.6, and controlling the concentration of the sodium molybdate in the solvent to be 0.02 g/ml;
(2) heating the mixed solution in the step (1) to 240 ℃ to carry out solvothermal reaction for 20 h;
(3) cooling the product obtained in the step (2), and then alternately centrifuging and washing the product by using water and ethanol for three times;
(4) carrying out ultrasonic blending and intercalation on the product obtained in the step (3) by using polyethylene glycol, wherein the adding mass of the polyethylene glycol is 100% of that of molybdenum disulfide, the ultrasonic frequency is controlled to be 440HZ during ultrasonic treatment, the time is 1h, then transferring to a freeze dryer, the temperature is controlled to be minus 40 ℃, and freeze drying is carried out for 12 hours;
(5) and (4) placing the sample in the step (4) into a tube furnace, controlling the heating rate to be 5 ℃ per minute, and heating to 800 ℃ for 2 hours to prepare the molybdenum disulfide intercalation material.
The foregoing description of specific embodiments of the present invention has been presented. It is to be understood that the present invention is not limited to the specific embodiments described above, and that various changes and modifications may be made by one skilled in the art within the scope of the appended claims without departing from the spirit of the invention.

Claims (7)

1. A preparation method of a molybdenum disulfide intercalation material is characterized by comprising the following steps:
(1) mixing sodium molybdate and thioacetamide, and adding a solvent for dissolving;
(2) heating the mixed solution in the step (1) to perform a solvothermal reaction;
(3) cooling the product obtained in the step (2) and then centrifuging and washing;
(4) taking linear macromolecules to carry out ultrasonic uniform mixing intercalation on the product obtained in the step (3), and then transferring the product to a freeze dryer for freeze drying;
(5) placing the sample in the step (4) into a tubular furnace for calcination to prepare a molybdenum disulfide intercalation material;
the linear polymer in the step (4) comprises polyethyleneimine or polyethylene glycol, and the mass of the linear polymer is 20% -100% of that of molybdenum disulfide; the calcination in the step (5) is controlled at the temperature of 600-800 ℃ for 2-6 hours, and the heating rate is 2-5 ℃ per minute.
2. The method for preparing a molybdenum disulfide intercalation material according to claim 1, wherein the mass ratio of sodium molybdate to thioacetamide in step (1) is 0.3-0.6: 0.6-1.2, and the solvent is a mixed solvent obtained by mixing water and ethylene glycol in a volume ratio of 2: 1.
3. The method for preparing a molybdenum disulfide intercalation material as claimed in claim 1, wherein the concentration of sodium molybdate in the solvent in step (1) is controlled to be 0.01-0.02 g/ml.
4. The method as claimed in claim 1, wherein the temperature of the solvothermal reaction in step (2) is 200-240 ℃ and the reaction time is 20-24 h.
5. The method for preparing the molybdenum disulfide intercalation material as claimed in claim 1, wherein the centrifugal washing in step (3) is three times of washing with water and ethanol alternately.
6. The method for preparing a molybdenum disulfide intercalation material as claimed in claim 1, wherein the ultrasonic mixing intercalation in step (4) has an ultrasonic frequency of 360-440HZ and a time of 1-3 h.
7. The method for preparing a molybdenum disulfide intercalation material as claimed in claim 1, wherein the freeze-drying in step (4) is controlled at-56-40 ℃ for 12-24 hours.
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