CN114613606B - M-MoS 2 @Ti 3 C 2 T x Heterostructure material and construction method and application thereof - Google Patents

M-MoS 2 @Ti 3 C 2 T x Heterostructure material and construction method and application thereof Download PDF

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CN114613606B
CN114613606B CN202210101150.6A CN202210101150A CN114613606B CN 114613606 B CN114613606 B CN 114613606B CN 202210101150 A CN202210101150 A CN 202210101150A CN 114613606 B CN114613606 B CN 114613606B
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CN114613606A (en
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王昕�
万峰
唐灿
李兵
张永兴
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Huaibei Normal University
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    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
    • H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
    • H01G11/22—Electrodes
    • H01G11/30—Electrodes characterised by their material
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
    • H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
    • H01G11/22—Electrodes
    • H01G11/24—Electrodes characterised by structural features of the materials making up or comprised in the electrodes, e.g. form, surface area or porosity; characterised by the structural features of powders or particles used therefor
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
    • H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
    • H01G11/22—Electrodes
    • H01G11/30—Electrodes characterised by their material
    • H01G11/32—Carbon-based
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
    • H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
    • H01G11/84—Processes for the manufacture of hybrid or EDL capacitors, or components thereof
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
    • H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
    • H01G11/84—Processes for the manufacture of hybrid or EDL capacitors, or components thereof
    • H01G11/86—Processes for the manufacture of hybrid or EDL capacitors, or components thereof specially adapted for electrodes
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    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
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    • Y02E60/13—Energy storage using capacitors

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Abstract

The invention discloses an M-MoS 2 @Ti 3 C 2 T x Heterostructure material, and construction method and application thereof, belongs to the technical field of electrochemical energy storage, and the construction method of the material comprises the following steps: urea, molybdenum trioxide, thioacetamide and Ti 3 C 2 T x Adding the mixture into water, and dissolving the mixture to obtain a reaction solution; transferring the reaction liquid into a reaction container for hydrothermal reaction, and naturally cooling to room temperature after the reaction is finished; taking out the solid precipitate in the reaction vessel, and washing and drying the solid precipitate in sequence to obtain solid powder, namely a final product. The invention adopts a one-step hydrothermal method to prepare the M-MoS with excellent electrochemical performance 2 @Ti 3 C 2 T x Heterostructure materials which have high specific capacitance, high rate performance, high cycle stability and other performances. The preparation method provided by the invention has the advantages of easily available raw materials, low cost and simple preparation process, and is suitable for industrial popularization and application.

Description

M-MoS 2 @Ti 3 C 2 T x Heterostructure material and construction method and application thereof
Technical Field
The invention belongs to the technical field of electrochemical energy storage, and in particular relates to an M-MoS 2 @Ti 3 C 2 T x Heterostructure materials, methods of construction and use thereof.
Background
Transition Metal Dichalcogenides (TMDs) are typically two-dimensional materials with special band structures, semiconducting or superconductive properties, etc. MoS (MoS) 2 As a representative member of TMD, the interlayer thereof is bonded by van der waals force, allowing intercalation of electrolyte ions, making it a hot spot material in the fields of supercapacitors, secondary batteries, electrocatalysis, and the like. MoS (MoS) 2 Is closely related to its crystal structure, there are mainly two typical crystal structures, respectively 2H semiconductor phases (S-MoS 2 ) And 1T metal phase (M-MoS) 2 )。S-MoS 2 The single layer bandgap of (2) is about 1.9eV, exhibiting semi-insulating properties that are detrimental to its use in supercapacitor electrode materials for energy storage. M-MoS 2 Ratio S-MoS 2 Has higher conductivity, shows metal characteristics, and has an interlayer spacing of about 0.95nm, about S-MoS 2 1.5 times (0.6 nm), which is favorable for obtaining more intercalation pseudo-capacitance and further shows high specific capacitance value. However, M-MoS 2 The specific capacitance value of (c) decreases rapidly with increasing current density, and the rate capability is poor. By M-MoS 2 And the material is compounded with a high-conductivity material to prepare a heterostructure, so that the rate performance of the heterostructure can be improved.
Transition metal carbo/nitrides (MXene) as novel two-dimensional materials of the general chemical formula M n+1 X n T x (e.g. Ti 3 C 2 MXene can also be written as Ti 3 C 2 T x ) Wherein T is x Surface functional groups (e.g., O, F and OH) of MXenes, ti 3 C 2 T x As the first reported MXene, it has ultra-high electron conductivity, reaching 150000S m -1 The electrode exhibits excellent rate performance and cycle stability when used as an electrode of a supercapacitor.
Thus, by assembling M-MoS 2 With Ti 3 C 2 T x Construction of M-MoS 2 @Ti 3 C 2 T x Heterostructures are expected to be able to obtain materials with high capacitance and high rate capability.
Disclosure of Invention
The invention aims to provide an M-MoS 2 @Ti 3 C 2 T x Heterostructure material, construction method and application thereof, so as to solve M-MoS in the prior art 2 Unstable performance and poor rate capability.
In order to achieve the above purpose, the invention adopts the following technical scheme:
M-MoS 2 @Ti 3 C 2 T x The construction method of the heterostructure material comprises the following steps:
(1) Reducing agent, molybdenum trioxide, sulfur source and Ti 3 C 2 T x Adding the mixture into water, and dissolving the mixture to obtain a reaction solution; preferably, the reducing agent is urea; the sulfur source is thioacetamide or sodium sulfide; the urea, molybdenum trioxide, thioacetamide and Ti 3 C 2 T x The mass ratio of (3) is 120:79:42: (4-10). The raw material molybdenum trioxide used in the invention is an orthorhombic system and contains octahedral MoO 6 The layered structure is favorable for preparing metal mold MoS containing Mo-S octahedral structure 2 (M-MoS 2 ) Thereby constructing M-MoS 2 @Ti 3 C 2 T x Heterostructures.
(2) Transferring the reaction liquid into a reaction container for hydrothermal reaction, and naturally cooling to room temperature after the reaction is finished; preferably, the reaction vessel is a high-pressure reaction kettle with a polytetrafluoroethylene lining; the temperature of the hydrothermal reaction is 160-220 ℃ and the time is 10-16h; specifically, the temperature of the hydrothermal reaction may be 160 ℃, 180 ℃, 200 ℃ or 220 ℃ for 10 hours, 12 hours, 14 hours or 16 hours.
(3) Taking out solid precipitate in the reaction vessel, washing and drying to obtain solid powder, namely M-MoS 2 /Ti 3 C 2 T x Heterostructure materials. Preferably, the washing method is to adopt deionized water and absolute ethyl alcohol to wash for several times respectively; the drying is carried out in a vacuum drying oven, and the drying temperature is 50-70 ℃.
The invention also discloses an electrode and a preparation method of the electrode, wherein the preparation method of the electrode comprises the following steps:
(1) Dispersing a binder, a conductive agent and an active material in an organic solvent to obtain slurry; the active material is M-MoS prepared by the method 2 @Ti 3 C 2 T x Heterostructure materials; preferably, the binder is PVDF, the conductive agent is acetylene black, and the organic solvent is NMP solution. Preferably, the current collector is carbon paper, the slurry coating area is controlled to be 1cm multiplied by 1cm,the coating quality is controlled to be about 1.5 mg.
(2) The slurry was coated on a current collector and dried to obtain an electrode.
It is another object of the present invention to disclose a supercapacitor comprising an electrode as described above.
The beneficial effects of the invention are as follows:
the invention adopts a simple one-step hydrothermal method to prepare the M-MoS with excellent electrochemical performance 2 @Ti 3 C 2 T x Heterostructure materials. The M-MoS 2 @Ti 3 C 2 T x When the heterostructure material is used as the anode material of the supercapacitor, the heterostructure material has good characteristics, such as: high specific capacitance, high rate performance, high cycling stability, etc. The invention has the advantages of easily obtained raw materials, low price and cost, low reaction temperature, almost no environmental pollution, no need of adding surfactant, easy separation of products, high purity of the obtained products, good and uniform appearance, simple preparation process and suitability for industrial popularization and application.
Drawings
FIG. 1 is a M-MoS prepared in example 1 2 @Ti 3 C 2 T x Heterostructure material and M-MoS prepared in comparative example 1 2 X-ray diffraction (XRD) patterns of (a);
FIG. 2 is a M-MoS prepared in comparative example 1 2 Scanning electron microscope photographs of (2);
FIG. 3 is a M-MoS prepared in example 1 2 @Ti 3 C 2 T x Heterostructure material and raw material Ti 3 C 2 T x Scanning Electron Microscope (SEM) photograph
FIG. 4 is a M-MoS prepared in example 1 2 @Ti 3 C 2 T x Heterostructure material and M-MoS prepared in comparative example 1 2 XPS profile (S2 p);
FIG. 5 is a M-MoS prepared in example 1 2 @Ti 3 C 2 T x Heterostructure material and M-MoS prepared in comparative example 1 2 XPS profile (Mo 3 d);
FIG. 6 shows the process of example 1The obtained M-MoS 2 @Ti 3 C 2 T x Raman spectra of heterostructure materials;
FIG. 7 is cyclic voltammograms of electrode 1 prepared in application example 1 at different scan rates;
FIG. 8 is a constant current charge-discharge curve of the electrode 1 prepared in application example 1 at different current densities;
FIG. 9 is a plot of the rate performance of electrode 1 and electrode 2 in a three electrode test system;
FIG. 10 is a test result of 5000 cycles of cycling stability of electrode 1 at a current density of 20A/g in a three electrode test system.
Detailed Description
The present invention will be further described with reference to examples, which are not intended to be limiting, so that those skilled in the art will better understand the present invention and practice it; the raw materials used in each of the following examples and comparative examples were commercially available products.
Example 1
M-MoS 2 @Ti 3 C 2 T x The preparation method of the heterostructure material comprises the following steps:
(1) Accurately weighing 1.2g of urea, 0.79g of molybdenum trioxide, 0.42g of thioacetamide and 0.06g of Ti 3 C 2 T x Dispersing the mixture in a beaker filled with 60mL of deionized water, and fully dissolving the mixture under the action of magnetic stirring to form a uniform solution to obtain a reaction solution.
(2) Transferring the reaction solution into a high-pressure reaction kettle with a polytetrafluoroethylene lining of which the capacity is 100mL, heating the reaction solution in an oven at the constant temperature of 200 ℃ for 12 hours, and naturally cooling the reaction solution to room temperature after the reaction is finished.
(3) Taking out black precipitate at the bottom of polytetrafluoroethylene lining, washing with deionized water and absolute ethanol for 3 times, and oven drying at 60deg.C in vacuum oven to constant weight to obtain black solid powder (M-MoS) 2 @Ti 3 C 2 T x Heterostructure materials.
Application example 1
A method of preparing an electrode comprising the steps of:
(5) 0.005g PVDF, 0.005g acetylene black and 0.04g M-MoS prepared in example 1 were weighed out 2 @Ti 3 C 2 T x Placing the heterostructure material into an agate mortar, dropwise adding 0.6ml of NMP solution, and fully grinding for 10min to obtain slurry;
(6) And uniformly coating the slurry on carbon paper, controlling the coating area to be 1cm multiplied by 1cm, placing the uniformly coated carbon paper in a vacuum drying oven, and drying at 60 ℃ until the weight is constant to obtain a corresponding electrode, which is denoted as electrode 1.
Comparative example 1
Compared with example 1, comparative example 1 differs in that: in the step (1), ti is not added 3 C 2 T x The other processes were the same as in example 1. Preparing M-MoS 2 A material.
Reference to the method for preparing electrode in application example 1, the product M-MoS prepared in comparative example 1 2 Material substitution M-MoS 2 @Ti 3 C 2 T x Heterostructure material, electrode 2, was prepared as well, and this was designated electrode 2.
Structural characterization and performance detection:
for M-MoS prepared in example 1 2 @Ti 3 C 2 T x Heterostructure materials and M-MoS made in comparative examples 2 The materials were characterized and the results are shown in figures 1-6.
FIG. 1 is a M-MoS prepared in example 1 2 @Ti 3 C 2 T x Heterostructure material and M-MoS prepared in comparative example 1 2 The lighter colored curve in FIG. 1 is M-MoS 2 @Ti 3 C 2 T x XRD profile of heterostructure material comprising two (002) characteristic diffraction peaks, located at 2θ=7.0° (Ti 3 C 2 T x (002) diffraction peak) and 2θ=9.0° (M-MoS) 2 (002) diffraction peak). Whereas pure M-MoS 2 Only one (002) diffraction peak was located at 2θ=9.0°. As can be seen from FIG. 1, M-MoS 2 @Ti 3 C 2 T x Heterostructure materials.
FIG. 2 is a M-MoS prepared in comparative example 1 2 From FIG. 2, it can be seen that the pure M-MoS is shown in the SEM photograph 2 Is a nanosheet.
FIG. 3 is a M-MoS prepared in example 1 2 @Ti 3 C 2 T x Heterostructure material (b) and raw material Ti 3 C 2 T x (a) Scanning electron microscope photographs of (2). (a) As can be seen from the figure, pure Ti 3 C 2 T x The surface of the micro-sheet is very clean. (b) The graph shows that the composition is shown in Ti 3 C 2 T x The surface uniformly grows a substance which is M-MoS as known by XRD in connection with figure one 2 Thus successfully preparing M-MoS 2 @Ti 3 C 2 T x Heterostructure materials.
Comparing FIG. 4 and FIG. 5, M-MoS 2 @Ti 3 C 2 T x Heterostructure material and pure M-MoS 2 The change in binding energy of S and Mo elements (-1.1 eV) in the alloy can prove M-MoS 2 @Ti 3 C 2 T x M-MoS in heterostructure materials 2 With Ti 3 C 2 T x Chemical bonding exists between the two.
M-MoS in FIG. 6 2 @Ti 3 C 2 T x Heterostructure material at 147cm -1 、235cm -1 、335cm -1 There appear three typical raman peaks J 1 、J 2 、J 3 Showing metal phase MoS 2 And at 280cm -1 Appear E 1g Raman peaks, demonstrating Mo at M-MoS 2 @Ti 3 C 2 T x Octahedral coordination in heterostructures further demonstrates that metal phase MoS in heterostructures 2 。
In the three-electrode test system, the electrodes 1 and 2 are subjected to electrochemical test, and the related conditions are as follows: the working electrode is an electrode 1 or an electrode 2, the reference electrode is an Ag/AgCl electrode, the counter electrode is a platinum sheet electrode, and the electrolyte is 1M sodium sulfate solution. The test results are shown in FIGS. 7-10.
Fig. 7 is a cyclic voltammogram of electrode 1 at different scan rates, which is rectangular-like in shape, showing that the electrode is a capacitive electrode material with a voltage window of-0.8-0.0V, which is a supercapacitor anode material.
Fig. 8 is a constant current charge-discharge curve of the electrode 1 at different current densities, the linear curve characteristics of which further demonstrate the capacitive behavior of the heterostructure.
Fig. 9 is a graph of the rate performance of the electrodes 1 and 2 in a three-electrode test system, and it is clear from fig. 9 that the specific capacitance values of the electrodes 1 and 2 are almost equal at a current density of 2A/g, but the specific capacitance value of the electrode 2 decreases rapidly with an increase in current density, and only the initial 39.4% of the specific capacitance value increases to 20A/g. While the specific capacitance value of the electrode 1 was still 75.75% of the initial value, showing excellent rate performance. The excellent electrochemical performance of the electrode 1 benefits from M-MoS 2 @Ti 3 C 2 T x Synergy of the components in the heterostructure material.
FIG. 10 is a graph showing the cycling stability of electrode 1 at a current density of 20A/g, showing that the capacity retention rate is as high as 95% by 5000 constant current charge and discharge tests, indicating M-MoS 2 @Ti 3 C 2 T x Heterostructure materials have excellent stability.
Example 2
(1) Accurately weighing 1.2g of urea, 0.79g of molybdenum trioxide, 0.42g of thioacetamide and 0.04g of Ti 3 C 2 T x Dispersing it in a beaker filled with 60mL deionized water, and fully dissolving it under the action of magnetic stirring to form a uniform solution.
(2) Transferring the uniform solution into a high-pressure reaction kettle with a polytetrafluoroethylene lining of 100mL capacity, heating the solution at a constant temperature in a baking oven of 200 ℃ for 12 hours, and naturally cooling to room temperature after the reaction is finished.
(3) Taking out black precipitate at the bottom of the polytetrafluoroethylene lining, and washing 3 times by deionized water and absolute ethyl alcohol respectively to obtain black solid powder.
Example 3
(1) Accurately weighing 1.2g of urea, 0.79g of molybdenum trioxide, 0.42g of thioacetamide and 0.08g of Ti 3 C 2 T x Dispersing it in a beaker filled with 60mL deionized water, and fully dissolving it under the action of magnetic stirring to form a uniform solution.
(2) Transferring the uniform solution into a high-pressure reaction kettle with a polytetrafluoroethylene lining of 100mL capacity, heating the solution at a constant temperature in a baking oven of 200 ℃ for 12 hours, and naturally cooling to room temperature after the reaction is finished.
(3) Taking out black precipitate at the bottom of the polytetrafluoroethylene lining, and washing 3 times by deionized water and absolute ethyl alcohol respectively to obtain black solid powder.
Example 4
(1) Accurately weighing 1.2g of urea, 0.79g of molybdenum trioxide, 0.42g of thioacetamide and 0.1g of Ti 3 C 2 T x Dispersing it in a beaker filled with 60mL deionized water, and fully dissolving it under the action of magnetic stirring to form a uniform solution.
(2) Transferring the uniform solution into a high-pressure reaction kettle with a polytetrafluoroethylene lining of 100mL capacity, heating the solution at a constant temperature in a baking oven of 200 ℃ for 12 hours, and naturally cooling to room temperature after the reaction is finished.
(3) Taking out black precipitate at the bottom of the polytetrafluoroethylene lining, and washing 3 times by deionized water and absolute ethyl alcohol respectively to obtain black solid powder.
Example 5
(1) Accurately weighing 1.2g of urea, 0.79g of molybdenum trioxide, 0.42g of thioacetamide and 0.06g of Ti 3 C 2 T x Dispersing it in a beaker filled with 40mL deionized water, and fully dissolving it under the action of magnetic stirring to form a uniform solution.
(2) Transferring the uniform solution into a high-pressure reaction kettle with a polytetrafluoroethylene lining of 100mL capacity, heating the solution at a constant temperature in a baking oven of 200 ℃ for 12 hours, and naturally cooling to room temperature after the reaction is finished.
(3) Taking out black precipitate at the bottom of the polytetrafluoroethylene lining, and washing 3 times by deionized water and absolute ethyl alcohol respectively to obtain black solid powder.
Example 6
(1) Accurately weighing 1.2g of urea, 0.79g of molybdenum trioxide, 0.42g of thioacetamide and 0.06g of Ti 3 C 2 T x Dispersing it in a beaker filled with 50mL of deionized water, and fully dissolving it under the action of magnetic stirring to form a uniform solution.
(2) Transferring the uniform solution into a high-pressure reaction kettle with a polytetrafluoroethylene lining of 100mL capacity, heating the solution at a constant temperature in a baking oven of 200 ℃ for 12 hours, and naturally cooling to room temperature after the reaction is finished.
(3) Taking out black precipitate at the bottom of the polytetrafluoroethylene lining, and washing 3 times by deionized water and absolute ethyl alcohol respectively to obtain black solid powder.
Example 7
(1) Accurately weighing 1.2g of urea, 0.79g of molybdenum trioxide, 0.42g of thioacetamide and 0.06g of Ti 3 C 2 T x Dispersing it in a beaker filled with 70mL deionized water, and fully dissolving it under the action of magnetic stirring to form a uniform solution.
(2) Transferring the uniform solution into a high-pressure reaction kettle with a polytetrafluoroethylene lining of 100mL capacity, heating the solution at a constant temperature in a baking oven of 200 ℃ for 12 hours, and naturally cooling to room temperature after the reaction is finished.
(3) Taking out black precipitate at the bottom of the polytetrafluoroethylene lining, and washing 3 times by deionized water and absolute ethyl alcohol respectively to obtain black solid powder.
Example 8
(1) Accurately weighing 1.2g of urea, 0.79g of molybdenum trioxide, 0.42g of thioacetamide and 0.06g of Ti 3 C 2 T x Dispersing it in a beaker filled with 60mL deionized water, and fully dissolving it under the action of magnetic stirring to form a uniform solution.
(2) Transferring the uniform solution into a high-pressure reaction kettle with a polytetrafluoroethylene lining of 100mL capacity, heating the solution at a constant temperature in an oven of 160 ℃ for 12 hours, and naturally cooling to room temperature after the reaction is finished.
(3) Taking out black precipitate at the bottom of the polytetrafluoroethylene lining, and washing 3 times by deionized water and absolute ethyl alcohol respectively to obtain black solid powder.
Example 9
(1) Accurately weighing 1.2g of urea, 0.79g of molybdenum trioxide, 0.42g of thioacetamide and 0.06g of Ti 3 C 2 T x Dispersing it in a beaker filled with 60mL deionized water, and fully dissolving it under the action of magnetic stirring to form a uniform solution.
(2) Transferring the uniform solution into a high-pressure reaction kettle with a polytetrafluoroethylene lining of 100mL capacity, heating the solution at a constant temperature in an oven of 180 ℃ for 12 hours, and naturally cooling to room temperature after the reaction is finished.
(3) Taking out black precipitate at the bottom of the polytetrafluoroethylene lining, and washing 3 times by deionized water and absolute ethyl alcohol respectively to obtain black solid powder.
Example 10
(1) Accurately weighing 1.2g of urea, 0.79g of molybdenum trioxide, 0.42g of thioacetamide and 0.06g of Ti 3 C 2 T x Dispersing it in a beaker filled with 60mL deionized water, and fully dissolving it under the action of magnetic stirring to form a uniform solution.
(2) Transferring the uniform solution into a high-pressure reaction kettle with a polytetrafluoroethylene lining of 100mL capacity, heating the solution at a constant temperature in an oven of 220 ℃ for 12 hours, and naturally cooling to room temperature after the reaction is finished.
(3) Taking out black precipitate at the bottom of the polytetrafluoroethylene lining, and washing 3 times by deionized water and absolute ethyl alcohol respectively to obtain black solid powder.
Through verification of the products prepared in the examples and the comparative examples, when the water consumption is changed in the preparation process, the volume of the air column in the reaction kettle is changed, which affects the pressure in the reaction kettle in the hydrothermal reaction, and further affects the structure of the final product; in addition, when Ti is changed 3 C 2 T x The amount of (C) also has an effect on the electrochemical properties of the final product, and the invention obtains proper Ti through experiments 3 C 2 T x Is used in the amount of (3)The prepared product has good specific capacitance and excellent multiplying power performance.
It will be apparent that the described embodiments are some, but not all, embodiments of the invention. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.

Claims (7)

1. M-MoS 2 @Ti 3 C 2 T x The construction method of the heterostructure material is characterized by comprising the following steps of: the method comprises the following steps:
(1) Reducing agent, molybdenum trioxide, sulfur source and Ti 3 C 2 T x Adding the mixture into water, and dissolving the mixture to obtain a reaction solution; the reducing agent is urea; the sulfur source is thioacetamide or sodium sulfide; the urea, molybdenum trioxide, thioacetamide and Ti 3 C 2 T x The mass ratio of (3) is 120:79:42: (4-10);
(2) Transferring the reaction liquid into a reaction container for hydrothermal reaction, and naturally cooling to room temperature after the reaction is finished; the temperature of the hydrothermal reaction is 160-220 ℃ and the time is 10-16h;
(3) Taking out solid precipitate in the reaction vessel, washing and drying to obtain solid powder, namely M-MoS 2 @Ti 3 C 2 T x Heterostructure materials.
2. The M-MoS of claim 1 2 @Ti 3 C 2 T x The construction method of the heterostructure material is characterized by comprising the following steps of: in the step (2), the reaction vessel is a high-pressure reaction kettle with a polytetrafluoroethylene lining.
3. The M-MoS of claim 1 2 @Ti 3 C 2 T x The construction method of the heterostructure material is characterized by comprising the following steps of: in the step (3), the washing method is to adopt deionized water and absolute ethyl alcohol to wash for several times respectively; the drying is carried out in a vacuum drying ovenThe drying is carried out at a temperature of 50-70 ℃.
4. M-MoS 2 @Ti 3 C 2 T x Heterostructure material, characterized in that: the M-MoS 2 @Ti 3 C 2 T x Heterostructure material is produced by a construction method according to any one of claims 1 to 3.
5. A method for preparing an electrode, characterized by: the method comprises the following steps:
(1) Dispersing a binder, a conductive agent and an active material in an organic solvent to obtain slurry; the active material being M-MoS as claimed in claim 4 2 @Ti 3 C 2 T x Heterostructure materials;
(2) The slurry was coated on a current collector and dried to obtain an electrode.
6. An electrode, characterized by: the electrode is prepared by the preparation method according to claim 5.
7. A supercapacitor, characterized in that: the supercapacitor comprises an electrode according to claim 6.
CN202210101150.6A 2022-01-27 2022-01-27 M-MoS 2 @Ti 3 C 2 T x Heterostructure material and construction method and application thereof Active CN114613606B (en)

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