CN110776012B - Preparation method of transition metal chalcogen layered compound nanosheet material - Google Patents
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Abstract
The invention discloses a preparation method of a transition metal chalcogenide layered compound nanosheet material, which combines an electrochemical intercalation method with a mechanical physical stripping method, adopts two conductive material interlayers to manufacture an electrochemical reaction electrode, introduces a material flowing system, carries out electrochemical intercalation in a water system and physically strips in a water-organic solvent mixed solvent system with proper surface tension to prepare a few layers of transition metal chalcogenide layered nanomaterial, can be carried out under the conditions of normal temperature and normal pressure, and has the advantages of high yield of obtained products, less residual quantity of intercalating agent, less residual un-stripped raw material amount, high purity of the products and better preparation efficiency than the traditional electrochemical method and organic solvent liquid phase stripping method.
Description
Technical Field
The invention belongs to the technical field of preparation of few-layer nano materials, and particularly relates to a preparation method of a transition metal chalcogenide layered compound nanosheet material.
Background
The transition metal chalcogenide layered compound material mainly comprises molybdenum disulfide, tungsten disulfide, molybdenum diselenide, molybdenum ditelluride, thallium diselenide, niobium diselenide, nickel ditelluride and the like. Once these transition metal chalcogenide layered compounds can be exfoliated into two-dimensional lamellar nanomaterials, they have shown numerous important applications in the fields of electronics, photovoltaics, and energy storage.
Molybdenum disulfide in the bulk phase is a typical transition metal chalcogenide layered structure material. It can be conveniently extracted and prepared from natural molybdenite and has been applied to the fields of lubrication, catalysis, composite materials and the like. The single-layer molybdenum disulfide sheet layer is formed by wrapping a molybdenum atom by an upper sulfur atom and a lower sulfur atomThe sandwich structure of the layer is about 0.8-1.0 nm in thickness. The in-plane electron mobility of the molybdenum disulfide lamella can reach 200-500 cm2Has a V.s value of up to 108The current switching ratio of the high-voltage power supply has very wide application prospect in various fields of flexible electronics, energy storage (lithium ion batteries, super capacitors and solar batteries), industrial catalysis and the like.
In recent years, with the intensive development of single-layer or few-layer two-dimensional nanomaterial preparation methods and application research, more and more researchers are working on developing low-cost and high-efficiency methods for massively preparing two-dimensional transition metal chalcogenide lamellar nanomaterials. The technical scheme disclosed in CN104495935B proposes that a molybdenum disulfide nanosheet material with a high yield is obtained by adding an oxidant in an organic solvent through stirring or ultrasonic methods, but the method easily causes the defect of a nanosheet layer, has a long preparation period, and is difficult to implement on a large scale. The technical scheme disclosed in CN106086919A adopts sulfate as electrolyte, and prepares the molybdenum disulfide nano material by an electrochemical method, but the method is to make the molybdenum disulfide and metals such as Ni, Cu, Fe, Co, Ag, etc. in a certain proportion into a composite material by dry pressing to be used as an anode, and metal or graphite as a cathode. The method can introduce metal ions with uncontrollable content into the product, and the metal ions cannot be completely removed, so that the product is impure and the application is influenced. The technical scheme disclosed in US20190143286a1 is to prepare a two-dimensional nanomaterial dispersion by a liquid phase exfoliation method, which mainly proposes some conductive molecules with special structures as excellent dispersants. The technical scheme disclosed in CN107720825A adopts magnesium chloride and sodium sulfide as intercalation agents, and molybdenum disulfide nanosheets are obtained by continuous heating and ultrasonic stripping in a high-pressure reaction kettle, but the method is high in energy consumption, low in yield and not suitable for large-scale preparation. Some researchers adopt a lithium ion chemical intercalation method combined with an ultrasonic stripping method to obtain nanosheets such as molybdenum disulfide, tungsten disulfide and the like, but the method is harsh in preparation conditions and complicated in preparation process, and the popularization and application of the method are limited. In a word, the existing preparation technology of transition metal chalcogen family flaky nanometer materials such as molybdenum disulfide still has the problems of long preparation period, high energy consumption, low yield, low purity and the like.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provides a preparation method of a transition metal chalcogenide layered compound nanosheet material.
The technical scheme of the invention is as follows:
a preparation method of a transition metal chalcogen layered compound nanosheet material comprises the following steps:
(1) uniformly mixing powder of transition metal chalcogen compound with the average grain diameter of 5-50um and a modifier in a weight ratio of 1: 0.01-10 to obtain a powder mixture, wherein the modifier comprises a micromolecular surfactant containing pyrrole groups or amino groups;
(2) preparing an electrolyte aqueous solution with a concentration of 0.01-40mg/mL (preferably 1-20mg/mL), wherein the electrolyte comprises strong base, strong acid, strong base weak acid salt, weak acid strong base salt, weak acid salt with organic modification groups and weak base salt with organic modification groups;
(3) uniformly dispersing the powder mixture into the electrolyte aqueous solution to obtain first slurry, wherein the concentration of the transition metal chalcogen group powder in the first slurry is not lower than 1g/mL (preferably 1-10 g/mL);
(4) placing the first slurry in an electrochemical reaction device for electrochemical intercalation reaction to obtain a second slurry containing an intercalation reaction product, wherein the first slurry is always ensured to be in a uniform flow exchange state in the reaction process;
The electrochemical reaction device comprises a direct current stabilized voltage power supply, a reaction cell and an electrode assembly, wherein the reaction cell is made of a first conductive material, and the outer surface of the first conductive material of the reaction cell is coated with a second conductive material; the electrode assembly is made of a first conductive material, and the interior of the electrode assembly is filled with a second conductive material; the anode of the direct current stabilized power supply is electrically connected with the second conductive material of the electrode assembly, and the cathode of the direct current stabilized power supply is electrically connected with the second conductive material of the reaction tank; the first conductive material is titanium, tungsten, steel, cast iron, titanium alloy, tungsten alloy or stainless steel, and the second conductive material is at least one of graphite, carbon, gold, silver, copper, aluminum, iron and tin;
the first slurry is placed in the reaction cell, and the electrode assembly is placed in the first slurry and does not contact with the inner surface of the reaction cell;
the output voltage of the direct current stabilized power supply is 1-100V, the load output current is 0.01-40A, the temperature of the electrochemical intercalation reaction is 0-100 ℃, and the time is 0.1-48 h;
(5) adding the second slurry with surface energy of 30-50 mJ.m-2Uniformly mixing the organic solvent to obtain third slurry, and then carrying out physical stripping treatment on the third slurry; the molar ratio of the organic solvent to the water in the electrolyte aqueous solution in the step (2) is 0.001-0.5: 1, and the concentration of the intercalation reaction product in the third slurry is 10g/L-1000 g/L;
(6) And (4) centrifuging the material obtained in the step (5) at a low speed to remove large particles which are not completely stripped, repeatedly washing the upper thick slurry by using ethanol and deionized water for many times in a vacuum filtration mode, and drying to obtain the transition metal chalcogen layered compound nanosheet material.
In a preferred embodiment of the present invention, the method for ensuring that the first slurry is in a uniform flow exchange state during the reaction of step (4) is to add a stirring or flowing system, and further preferably a uniform stirring system or a peristaltic circulating system.
In a preferred embodiment of the present invention, the physical stripping treatment in the step (5) is high-speed shear emulsification, high-energy ball milling or ultrasonic treatment, and further preferably, the ultrasonic treatment is treatment with an ultrasonic cleaning machine, an ultrasonic shaker or a probe type ultrasonic cell crusher.
In a preferred embodiment of the present invention, the modifier comprises at least one of polyvinylpyrrolidone, polyethylene glycol, sodium dodecylbenzenesulfonate, tween 80, sodium cholate, dodecyltrimethylammonium bromide, and hexadecyltrimethylammonium bromide.
In a preferred embodiment of the present invention, the electrolyte includes at least one of potassium hydroxide, sodium hydroxide, sulfuric acid, nitric acid, chlorosulfonic acid, phosphoric acid, hydrogen peroxide, ammonia water, sodium bicarbonate, potassium bicarbonate, ammonium bisulfate, sodium bisulfate, tetraethylammonium bromide, tetrabutylammonium bromide, tetraethylammonium bisulfate, tetrabutylammonium bisulfate, dodecyltrimethylammonium bromide, and hexadecyltrimethylammonium bromide.
In a preferred embodiment of the invention, the inner surface of the reaction cell is provided with a coating comprising precious metals including ruthenium, iridium, platinum, zinc, tin.
In a preferred embodiment of the present invention, the outer surface of the electrode assembly has a plating layer containing a noble metal including ruthenium, iridium, platinum, zinc, tin.
In a preferred embodiment of the present invention, the organic solvent in the step (5) comprises benzyl benzoate, N-methylpyrrolidone, N-cyclohexylpyrrolidone, N-dimethylformamide, dimethyl sulfoxide, cyclohexane and a mixture of ethanol and deionized water.
In a preferred embodiment of the invention, the transition metal chalcogenides include molybdenum disulfide, tungsten disulfide, molybdenum diselenide, molybdenum ditelluride, thallium diselenide, niobium diselenide, and nickel ditelluride.
The beneficial effects of the invention are:
1. the thickness of the transition metal chalcogen layered compound nanosheet material prepared by the method is 1nm-30nm, the oxygen content is less than 2 at%, the nitrogen content is less than 5 at%, and the characteristic absorption peak range of the main ultraviolet absorption spectrum is 400-700nm, so that the transition metal chalcogen layered compound nanosheet material can be applied to a hole transport layer material of a photoelectric device, can also be applied to a basic material of a logic switch electronic component, a novel transistor, a battery, a hot electron device and a superconducting composite material, can be used independently, and can also be compounded with other materials for use.
2. The invention combines an electrochemical intercalation method and a mechanical physical stripping method, adopts two conductive material interlayers to manufacture an electrochemical reaction electrode, introduces a material flowing system, carries out electrochemical intercalation in a water system and physically strips in a water-organic solvent mixed solvent system with proper surface tension to prepare few layers of transition metal chalcogen layered nano materials, can be carried out under the conditions of normal temperature and normal pressure, and has the advantages of high yield of obtained products, less residual quantity of intercalation agent, less residual un-stripped raw material amount, high product purity and better preparation efficiency than the traditional electrochemical method and organic solvent liquid phase stripping method.
3. The preparation process is low in cost and environment-friendly, and the product can be applied to photoelectric and electronic devices, is suitable for large-scale production and has high popularization value.
Drawings
Fig. 1 is a transmission electron microscope image of the few-layer molybdenum disulfide nano material prepared in example 2 of the present invention.
Fig. 2 is a local high-resolution tem image of the few-layer mo disulfide nanomaterial prepared in example 2 of the present invention.
Fig. 3 is a graph of the ultraviolet absorption spectrum of the few-layer molybdenum disulfide nano material prepared in embodiments 1 to 3 (corresponding to # 1, # 2 and # 3, respectively) of the present invention.
Detailed Description
The technical solution of the present invention will be further illustrated and described below with reference to the accompanying drawings by means of specific embodiments.
The electrochemical reaction device in the following embodiments comprises a DC stabilized voltage power supply, a reaction cell and an electrode assembly, wherein the reaction cell is made of a first conductive material, and the outer surface of the first conductive material of the reaction cell is coated with a second conductive material; the electrode assembly is made of a first conductive material, and the inside of the electrode assembly is filled with a second conductive material; the anode of the direct current stabilized power supply is electrically connected with the second conductive material of the electrode assembly, and the cathode of the direct current stabilized power supply is electrically connected with the second conductive material of the reaction tank; the first conductive material is titanium, tungsten, steel, cast iron, titanium alloy, tungsten alloy or stainless steel, and the second conductive material is at least one of graphite, carbon, gold, silver, copper, aluminum, iron and tin;
the slurry is placed in a reaction cell, and the electrode assembly is placed in the first slurry without contacting the inner surface of the reaction cell.
Example 1
(1) Molybdenum disulfide powder with the average particle size of 10um and polyvinylpyrrolidone (K30) are mixed by a mixing ratio of 98: 2 to obtain 30.6g of powder mixture;
(2) Preparing 20mL of electrolyte aqueous solution with the concentration of 8mg/mL, wherein the electrolyte is ammonium bicarbonate;
(3) uniformly dispersing the powder mixture in the electrolyte aqueous solution to obtain first slurry;
(4) placing the first slurry in an electrochemical reaction device for electrochemical intercalation reaction to obtain a second slurry containing an intercalation reaction product, introducing a square track uniform-speed stirring system in the reaction process, and always ensuring that the first slurry is in a uniform flow exchange state;
the electrochemical reaction device comprises a direct current stabilized voltage power supply, a reaction tank and an electrode assembly, wherein the reaction tank is a cuboid, is made of metal titanium, has the size of 50mm multiplied by 30mm multiplied by 20mm, and is coated with red copper on the outer surface; the size of the electrode assembly is 20mm multiplied by 10mm multiplied by 20mm, the electrode assembly is made of metal titanium, and the inner part of the electrode assembly is filled with red copper; the anode of the direct current stabilized power supply is electrically connected with the red copper part of the electrode assembly, and the cathode of the direct current stabilized power supply is electrically connected with the red copper part of the reaction tank; the inner surface of the reaction cell and the outer surface of the electrode assembly are both provided with ruthenium coatings;
the first slurry is placed in the reaction cell, and the electrode assembly is placed in the first slurry and does not contact with the inner surface of the reaction cell;
The output voltage of the direct current stabilized power supply is 60V, the load output current is 0.5-4A, the temperature of electrochemical intercalation reaction is 25 ℃, and the time is 6 h;
(5) placing the second slurry in a stripping beaker, adding 50mL of N-methylpyrrolidone (NMP) into the stripping beaker, uniformly mixing to obtain a third slurry, and then carrying out stripping treatment on the third slurry at the rotating speed of 2500rpm by adopting high-speed shearing emulsification;
(6) and (3) centrifuging the material obtained in the step (5) at a low speed of 2000rpm to remove large particles which are not completely peeled, repeatedly washing the thick slurry on the upper layer by using ethanol and deionized water for multiple times in a vacuum filtration mode, and then drying in vacuum to obtain the final few-layer molybdenum disulfide nano material with the thickness of 10-20nm, wherein as shown in figure 3, an ultraviolet absorption spectrogram has obvious absorption peaks near 612nm and 647nm, and the two peaks are characteristic peaks of a molybdenum disulfide direct band gap semiconductor, which indicates that a plurality of single-layer or few-layer molybdenum disulfide nanosheets exist in the sample.
Example 2
(1) Uniformly mixing molybdenum disulfide powder with the average particle size of 20 mu m and polyethylene glycol (the relative molecular mass is 1500g/mol) according to the weight ratio of 99: 1 to obtain 30.3g of powder mixture;
(2) preparing 20mL of electrolyte aqueous solution with the concentration of 5mg/mL, wherein the electrolyte is hydrogen peroxide;
(3) Uniformly dispersing the powder mixture in the electrolyte aqueous solution to obtain first slurry;
(4) placing the first slurry in an electrochemical reaction device for electrochemical intercalation reaction to obtain a second slurry containing an intercalation reaction product, introducing a square track uniform-speed stirring system in the reaction process, and always ensuring that the first slurry is in a uniform flow exchange state;
the electrochemical reaction device comprises a direct current stabilized voltage power supply, a reaction tank and an electrode assembly, wherein the reaction tank is a cuboid and is made of metal titanium, the size of the reaction tank is 50mm multiplied by 30mm multiplied by 20mm, and the outer surface of the reaction tank is coated with red copper; the size of the electrode assembly is 20mm multiplied by 10mm multiplied by 20mm, the electrode assembly is made of metal titanium, and the interior of the electrode assembly is filled with red copper; the anode of the direct current stabilized power supply is electrically connected with the red copper part of the electrode assembly, and the cathode of the direct current stabilized power supply is electrically connected with the red copper part of the reaction tank; the inner surface of the reaction cell and the outer surface of the electrode assembly are both provided with ruthenium coatings;
the first slurry is placed in the reaction cell, and the electrode assembly is placed in the first slurry and does not contact with the inner surface of the reaction cell;
the output voltage of the direct current stabilized power supply is 40V, the load output current is 1-5A, the temperature of the electrochemical intercalation reaction is 25 ℃, and the time is 8 h;
(5) Placing the second slurry in a stripping beaker, adding 50mL of N, N-dimethylformamide into the stripping beaker, uniformly mixing to obtain a third slurry, and then carrying out stripping treatment on the third slurry at the rotating speed of 2500rpm by adopting high-speed shearing emulsification;
(6) and (3) centrifuging the material obtained in the step (5) at a low speed of 2000rpm to remove large particles which are not completely peeled, repeatedly washing the upper thick slurry by using ethanol and deionized water for many times in a vacuum filtration mode, and then drying the slurry in vacuum to obtain the final molybdenum disulfide nano material with a small layer thickness of 1-15m, wherein the thickness of most lamellar materials is about 10nm, and the thickness of a small number of lamellar materials is about 2-3nm, as shown in figures 1 and 2. As shown in the curve No. 2 of figure 3, the ultraviolet absorption spectrum of the material water dispersion liquid shows remarkable absorption peaks near 612nm and 647nm, and the two peaks are characteristic peaks of a molybdenum disulfide direct band gap semiconductor and indicate the existence of a single layer or few layers of molybdenum disulfide nanosheets.
Example 3
(1) Molybdenum disulfide powder with the average particle size of 30um and dodecyl trimethyl ammonium bromide are mixed according to the weight ratio of 98: 2 to obtain 30.6g of powder mixture;
(2) preparing 15mL of electrolyte aqueous solution with the concentration of 12.5mg/mL, wherein the electrolyte is ammonium bisulfate;
(3) Uniformly dispersing the powder mixture in the electrolyte aqueous solution to obtain first slurry;
(4) placing the first slurry in an electrochemical reaction device for electrochemical intercalation reaction to obtain a second slurry containing an intercalation reaction product, introducing a stirring system with uniform-speed circular motion in the reaction process, and always ensuring that the first slurry is in a uniform flow exchange state;
the electrochemical reaction device comprises a direct current stabilized voltage power supply, a reaction tank and an electrode assembly, wherein the reaction tank is cylindrical and is made of stainless steel, the height of the reaction tank is 100mm, the diameter of the reaction tank is 45mm, and the outer surface of the reaction tank is coated with aluminum; the electrode assembly is cylindrical, 100mm in height and 15mm in diameter, is made of stainless steel, and is filled with aluminum; the anode of the direct current stabilized power supply is electrically connected with the aluminum part of the electrode assembly, and the cathode of the direct current stabilized power supply is electrically connected with the aluminum part of the reaction tank; the inner surface of the reaction cell and the outer surface of the electrode assembly are both provided with ruthenium coatings;
the first slurry is placed in the reaction cell, and the electrode assembly is placed in the first slurry and does not contact with the inner surface of the reaction cell;
the output voltage of the direct current stabilized power supply is 30V, the load output current is 0.5-3A, the temperature of electrochemical intercalation reaction is 25 ℃, and the time is 10 h;
(5) Placing the second slurry in a stripping beaker, adding 40mL of N, N-dimethylformamide into the stripping beaker, uniformly mixing to obtain a third slurry, and then carrying out stripping treatment on the third slurry at the rotating speed of 2500rpm by adopting high-speed shearing emulsification;
(6) and (3) centrifuging the material obtained in the step (5) at a low speed of 2000rpm to remove large particles which are not completely stripped, repeatedly washing the thick slurry on the upper layer by using ethanol and deionized water for multiple times in a vacuum filtration mode, and then drying in vacuum to obtain the final molybdenum disulfide nano material with a few layers and a thickness of 1-20nm, wherein as shown in a curve No. 3 in figure 3, the ultraviolet absorption spectrogram of the water dispersion of the material has obvious absorption peaks near 612nm and 647nm, and the two peaks are characteristic peaks of the direct band gap semiconductor material of molybdenum disulfide and indicate that more single-layer or few-layer molybdenum disulfide nano sheets exist in the sample.
Example 4
(1) Mixing molybdenum disulfide powder with the average particle size of 50um and polyvinylpyrrolidone (K30) according to the weight ratio of 100: 5 to obtain 105g of powder mixture;
(2) preparing 60mL of electrolyte aqueous solution with the concentration of 8mg/mL, wherein the electrolyte is tetraethylammonium bisulfate;
(3) uniformly dispersing the powder mixture in the electrolyte aqueous solution to obtain first slurry;
(4) Placing the first slurry in an electrochemical reaction device for electrochemical intercalation reaction to obtain a second slurry containing an intercalation reaction product, introducing a stirring system with uniform-speed circular motion in the reaction process, and always ensuring that the first slurry is in a uniform flow exchange state;
the electrochemical reaction device comprises a direct current stabilized voltage power supply, a reaction tank and an electrode assembly, wherein the reaction tank is cylindrical, is made of stainless steel, is 100mm high and 45mm in diameter, and is coated with aluminum on the outer surface; the electrode assembly is cylindrical, 100mm in height and 15mm in diameter, is made of stainless steel, and is filled with aluminum; the anode of the direct current stabilized power supply is electrically connected with the aluminum part of the electrode assembly, and the cathode of the direct current stabilized power supply is electrically connected with the aluminum part of the reaction tank; the inner surface of the reaction cell and the outer surface of the electrode assembly are both provided with ruthenium coatings;
the first slurry is placed in the reaction cell, and the electrode assembly is placed in the first slurry and does not contact with the inner surface of the reaction cell;
the output voltage of the direct current stabilized power supply is 35V, the load output current is 1-3.5A, the temperature of the electrochemical intercalation reaction is 25 ℃, and the time is 12 h;
(5) placing the second slurry in a stripping beaker, adding 80mL of N-methyl pyrrolidone into the stripping beaker, uniformly mixing to obtain a third slurry, and then carrying out stripping treatment on the third slurry at the rotating speed of 2500rpm by adopting high-speed shearing emulsification;
(6) And (3) centrifuging the material obtained in the step (5) at a low speed of 2000rpm to remove large particles which are not completely peeled, repeatedly washing the thick slurry on the upper layer by using ethanol and deionized water in a vacuum filtration mode for many times, and then carrying out vacuum drying to obtain the final few-layer molybdenum disulfide nano material with the thickness of 1-10 nm.
The above description is only a preferred embodiment of the present invention, and therefore should not be taken as limiting the scope of the invention, which is defined by the appended claims.
Claims (5)
1. A preparation method of a transition metal chalcogen layered compound nanosheet material is characterized by comprising the following steps: the method comprises the following steps:
(1) uniformly mixing powder of a transition metal chalcogenide compound with the average particle size of 5-50um and a modifier in a weight ratio of 1:0.01-10 to obtain a powder mixture, wherein the modifier is at least one of polyvinylpyrrolidone, polyethylene glycol, dodecyl trimethyl ammonium bromide and hexadecyl trimethyl ammonium bromide;
(2) preparing an electrolyte aqueous solution with the concentration of 0.01-40mg/mL, wherein the electrolyte is at least one of tetraethylammonium bromide, tetrabutylammonium bromide, tetraethylammonium bisulfate, tetrabutylammonium bisulfate, dodecyltrimethylammonium bromide and hexadecyltrimethylammonium bromide;
(3) Uniformly dispersing the powder mixture into the electrolyte aqueous solution to obtain first slurry, wherein the concentration of the transition metal chalcogenide powder in the first slurry is not lower than 1 g/mL;
(4) placing the first slurry in an electrochemical reaction device for electrochemical intercalation reaction to obtain a second slurry containing an intercalation reaction product, wherein the first slurry is always ensured to be in a uniform flow exchange state in the reaction process;
the electrochemical reaction device comprises a direct current stabilized voltage power supply, a reaction cell and an electrode assembly, wherein the reaction cell is made of a first conductive material, and the outer surface of the first conductive material of the reaction cell is coated with a second conductive material; the electrode assembly is made of a first conductive material, and the interior of the electrode assembly is filled with a second conductive material; the anode of the direct current stabilized power supply is electrically connected with the second conductive material of the electrode assembly, and the cathode of the direct current stabilized power supply is electrically connected with the second conductive material of the reaction tank; the first conductive material is titanium, tungsten, cast iron, titanium alloy, tungsten alloy or stainless steel, and the second conductive material is at least one of graphite, gold, silver, copper, aluminum, iron and tin;
the first slurry is placed in the reaction cell, and the electrode assembly is placed in the first slurry and does not contact with the inner surface of the reaction cell;
The output voltage of the direct current stabilized power supply is 1-100V, the load output current is 0.01-40A, the temperature of the electrochemical intercalation reaction is 0-100 ℃, and the time is 0.1-48 h;
(5) adding the second slurry with surface energy of 30-50 mJ.m-2Uniformly mixing the organic solvent to obtain third slurry, and then carrying out physical stripping treatment on the third slurry; the molar ratio of the organic solvent to the water in the aqueous electrolyte solution in step (2) is 0.001-0.5:1, and the concentration of the intercalation reaction product in the third slurry isThe degree is 10g/L-1000 g/L;
(6) and (4) centrifuging the material obtained in the step (5) at a low speed to remove large particles which are not completely stripped, repeatedly washing the upper thick slurry by using ethanol and deionized water for many times in a vacuum filtration mode, and drying to obtain the transition metal chalcogen layered compound nanosheet material.
2. The method of claim 1, wherein: the inner surface of the reaction tank is provided with a coating layer containing noble metal, and the noble metal is at least one of ruthenium, iridium and platinum.
3. The method of claim 1, wherein: the outer surface of the electrode assembly has a plating layer containing a noble metal, which is at least one of ruthenium, iridium, and platinum.
4. The method of claim 1, wherein: the organic solvent in the step (5) is benzyl benzoate,N-methyl pyrrolidone,N-cyclohexylpyrrolidone,N,N-at least one of dimethylformamide, dimethylsulfoxide, cyclohexane.
5. The production method according to any one of claims 1 to 4, characterized in that: the transition metal chalcogen group includes molybdenum disulfide, tungsten disulfide, molybdenum diselenide, molybdenum ditelluride, thallium diselenide, niobium diselenide, and nickel ditelluride.
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