CN109666946B - Two-dimensional layered MoS prepared by molten salt electrochemical intercalation method2Method of producing a material - Google Patents
Two-dimensional layered MoS prepared by molten salt electrochemical intercalation method2Method of producing a material Download PDFInfo
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Abstract
Two-dimensional layered MoS prepared by molten salt electrochemical intercalation method2A method of material belongs to the technical field of molten salt electrochemical intercalation. The method comprises the following steps: and removing water in the molten salt raw material of the molten salt system, and heating the molten salt system until the molten salt is molten. After the constant temperature is stableUnder argon atmosphere, graphite anode and MoS are added2Putting the cathode plate into molten salt, and applying constant current of 25-100 mA for reaction to obtain MoS2After the cathode plate is cooled, repeatedly cleaning and centrifuging by deionized water, and drying to obtain the two-dimensional layered MoS2A material. Two-dimensional layered MoS prepared by adopting method2The material has the advantages of low cost, high yield, simple process flow, short time consumption, environmental friendliness and no influence of oxygen-containing functional groups.
Description
Technical Field
The invention relates to the technical field of molten salt electrochemical intercalation, in particular to a method for preparing two-dimensional layered MoS by a molten salt electrochemical intercalation method2A method of making a material.
Background
In recent years, two-dimensional semiconductor materials, because of their heterogeneous structures, have very good application prospects in various fields such as electricity, optics and clean energy, and thus attract more and more interests and researches of researchers. Since the first preparation of graphene, although great progress has been made, graphene is a zero band gap material, which limits its application in practical circuits. To use MoS2The two-dimensional transition metal chalcogenide material has good research value and application prospect in many fields such as flexible photoelectric detectors, optical switches, light emitters, information electronics, solar cells and the like due to the advantages of good flexibility, adjustable electronic height and the like. Thus preparing two-dimensional layered MoS2Materials are highly necessary. Preparation of two-dimensional layered MoS2The main methods of the material are as follows: mechanical exfoliation, liquid exfoliation, chemical, electrochemical ion intercalation and exfoliation, chemical vapor deposition. Although the two-dimensional layered MoS can be prepared by the methods2But all suffer from a number of drawbacks. For example, the mechanical exfoliation method has low yield and layered MoS2Is difficult to control, the precursor requires large-sized layered crystals, and the dependence on the substrate is large. The liquid exfoliation method has the disadvantages of low yield, small and uneven product, and the like. The chemical, electrochemical ion intercalation and exfoliation method limits the size and layer distribution of two-dimensional materials, and oxygen-containing functional groups in the electrolyteInfluence the two-dimensional layered MoS2The electrochemical performance of (2). The chemical vapor deposition method requires a high reaction temperature and a high demand for a tube furnace and a substrate used for growth. And the molten salt electrochemical intercalation method has the advantages of low cost, high yield, simple process flow, short time consumption, environmental friendliness and no influence of oxygen-containing functional groups.
Disclosure of Invention
Aiming at the problems in the prior art, the invention provides a method for preparing two-dimensional layered MoS by a molten salt electrochemical intercalation method2The method of preparing the material is to add NaCl-CaCl2Molten salt system, LiCl-KCl molten salt system, NaCl-KCl-MgCl2Molten salt system, NaCl-KCl-ZnCl2One of the molten salt systems, the molten salt system is heated until the molten salt melts. After the constant temperature is stable, the graphite anode and the MoS are put under the argon atmosphere2Putting the cathode plate into molten salt, and applying constant current to react to obtain MoS2After the cathode plate is cooled, repeatedly cleaning and centrifuging by deionized water, and drying to obtain the two-dimensional layered MoS2A material. The method of the invention is adopted to prepare the two-dimensional layered MoS2The material has the advantages of low cost, high yield, simple process flow, short time consumption, environmental friendliness and no influence of oxygen-containing functional groups.
The invention relates to a method for preparing two-dimensional layered MoS by using a molten salt electrochemical intercalation method2A method of making a material comprising the steps of:
step 1: preparation of
(1) Pretreatment of molten salt feedstock
Weighing the molten salt raw materials according to the molten salt raw material components of a molten salt system, respectively pretreating the molten salt raw materials in a vacuum state, removing water in the molten salt raw materials, and cooling to room temperature to obtain the dehydrated molten salt raw materials;
the molten salt system is one of mixed molten salt systems of chloride;
(2) preparation of the electrodes
Mixing MoS2Pressing the powder into electrode plate, sintering, and using as MoS2The cathode is fixed on the first molybdenum rod current collector by a fine molybdenum wire;
polishing, cleaning and drying the surface of the graphite rod to be used as a graphite anode and fixing the graphite anode on a second molybdenum rod current collector;
step 2: assembling reaction system
(1) Cleaning and drying the molten salt electrochemical reactor to obtain a dried molten salt electrochemical reactor;
(2) mixing the dehydrated molten salt raw materials according to a molten salt system, adding the mixture into a crucible after mixing, and sealing the crucible in a dried molten salt electrochemical reactor;
(3) placing the sealed molten salt electrochemical reactor in a muffle furnace, heating to 200-500 ℃ in a vacuum state, preserving heat for 3-5 h, introducing Ar as protective gas, continuously heating to a temperature not lower than the melting temperature of a molten salt system of 50-100 ℃, keeping the temperature for 0-30min, and electrolyzing;
(4) graphite anode and MoS2Inserting a cathode into a molten salt system, applying a constant current of 25-100 mA, electrolyzing for 0.5-6 h, and carrying out MoS2Taking out the cathode, and cooling to obtain the electrolyzed MoS2A cathode;
and step 3: post-treatment
The electrolyzed MoS2Cathode, soaking in deionized water to remove MoS2Dissolving the molten salt attached to the surface and the interior of the cathode to obtain black MoS2Suspending liquid;
mixing black MoS2Repeatedly centrifuging and ultrasonically washing the suspension to obtain MoS2Vacuum drying the solid product to obtain two-dimensional layered MoS2A material.
In the step 1(1), the molten salt raw material is ground before pretreatment to obtain the molten salt raw material with the particle size less than or equal to 2 mm.
In the step 1(1), the molten salt system is NaCl-CaCl2Molten salt system, LiCl-KCl molten salt system, NaCl-KCl-MgCl2Molten salt system, NaCl-KCl-ZnCl2One of molten salt systems.
The NaCl-CaCl2In a molten salt system, the molar ratio of NaCl: CaCl2＝0.479：0.521；
In the LiCl-KCl molten salt system, the molar ratio of LiCl: KCl ═ 0.592: 0.408 of;
in the NaCl-KCl molten salt system, the molar ratio of NaCl: KCl ═ 0.5: 0.5;
the NaCl-KCl-MgCl2In a molten salt system, the molar ratio of NaCl: KCl: MgCl2＝0.33：0.216：0.454；
The NaCl-KCl-ZnCl2In a molten salt system, the molar ratio of NaCl: KCl: ZnCl2＝0.2：0.2：0.6。
In the step 1(1), the molten salt raw material is NaCl and CaCl2、LiCl、KCl、MgCl2、ZnCl2The specific components are determined according to the selected molten salt system.
In the step 1(1), the pretreatment is: heating to 200-350 ℃, keeping the temperature for 5-10 h, wherein the heating rate is 2-5 ℃/min.
In the step 1 and the step 2, the electrode plate has a diameter of 16mm and a thickness of 2.8-3 mm.
In the step 1(2), the pressing pressure is 4-5 MPa.
In the step 1(2), the sintering is specifically sintering at 800-900 ℃ for 4-6 h in Ar atmosphere.
In the step 1(2), the fine molybdenum wire is a fine molybdenum wire with a diameter of 0.18 mm.
In the step 1(2), the graphite rod has a diameter of 10mm and a length of 100 mm.
In the step 1(2), the first molybdenum rod current collector is a molybdenum rod with the diameter of 1.5mm and the length of 1.2 m; the second molybdenum rod current collector is a molybdenum rod with the diameter of 1.5mm and the length of 1.2 m.
In the step 1(2), the grinding is to remove impurities on the surface of the graphite rod by using 400-mesh sand paper; the cleaning is carried out by adopting alcohol.
In the step 1(2), a hole is formed at one end of the graphite rod, and the molybdenum rod current collector is inserted into the hole for fixing, wherein the diameter of the hole is 1.5mm, and the depth of the hole is 10 mm.
And in the step 2(1), the cleaning and drying are carried out, specifically, the cleaning and drying are carried out repeatedly by using water, then the drying is carried out naturally, and then the drying is carried out in a muffle furnace to be heated to 100-120 ℃, the heating rate is 2-3 ℃/min, and the constant temperature is 20-60 min.
In the step 2 and the step 3, the temperature is raised to 200-500 ℃, and the temperature raising rate is 3-5 ℃/min.
In the step 2 and the step 3, the temperature is continuously increased to be more than or equal to 50-100 ℃ of the melting temperature of the molten salt system, and the temperature increase rate is 3-5 ℃/min.
In the step 2(3), the melting temperature is preferably 350-850 ℃.
In the step 2(3), Ar gas is introduced as a protective gas, and the flow rate of Ar is 80-150 mL/min.
In the step 3, the soaking is to mix MoS2And (4) completely soaking, wherein the preferred soaking time is 10-15 h.
In the step 3, the centrifugation is carried out at a centrifugation rotating speed of 8000-12000 r/min for 5-10 min.
In the step 3, the vacuum drying is carried out at the drying temperature of 50-70 ℃ for 10-15 h.
The molten salt electrochemical intercalation method of the invention is used for preparing two-dimensional layered MoS2Method of producing a material based on MoS2Is a layered substance, the layers are connected with each other by weak van der Waals force, and cations can be intercalated into MoS in the electrolytic process2Between layers, the layers are separated, and in the post-treatment, the ultrasonic process makes the separated layered MoS2The dispersion is more thorough.
The invention relates to a method for preparing two-dimensional layered MoS by using a molten salt electrochemical intercalation method2The method for preparing the material has the beneficial effects that:
1. the traditional method for preparing the two-dimensional material has low yield, strict requirements on precursors and large dependence on substrates. The invention prepares two-dimensional MoS by electrochemical intercalation in molten salt2The material has relatively large yield, low requirement on the precursor and no need of substrate support.
2. Two-dimensional MoS prepared by adopting existing chemical, electrochemical ion intercalation and exfoliation methods2When the material is prepared, oxygen-containing functional groups in the electrolyte can influence the two-dimensional layered MoS2The electrochemical performance of (2). The invention prepares two-dimensional MoS by electrochemical intercalation in molten salt2The material, because the molten salt is carried out under the oxygen-free condition, has no influence of oxygen-containing functional groups, and can improve MoS2The electrochemical performance of (2).
3. The method has the advantages of low cost, high yield, simple process flow, short time consumption, environmental friendliness and no influence of oxygen-containing functional groups.
Drawings
FIG. 1 shows that the molten salt electrochemical intercalation method of the invention prepares two-dimensional layered MoS2Reaction apparatus diagram of materials.
Detailed Description
The present invention will be described in further detail with reference to examples.
In the following examples, unless otherwise specified, the equipment and starting materials used are commercially available and the chemical reagents are of greater than analytical purity.
In the following examples, the constant current is controlled by the constant current output from the novice system.
In the following examples, the molten salt electrochemical intercalation method is used to prepare two-dimensional layered MoS2The reaction apparatus for the materials is shown in FIG. 1.
Example 1
Two-dimensional layered MoS prepared by molten salt electrochemical intercalation method2The method of the material comprises the following steps:
in this example, the molten salt used was a chloride molten salt, specifically, NaCl — CaCl2In molar ratio, NaCl: CaCl2＝0.479：0.521。
Step 1: preparation of
(1) NaCl and CaCl2Pretreatment of salt
Weighing NaCl and CaCl according to the proportion of molten salt raw materials2NaCl and CaCl2Grinding respectively to obtain NaCl with particle size of 2mm andCaCl2grinding, pouring into beakers respectively, and placing in a muffle furnace for sealing;
heating the muffle furnace to 200 ℃ at a heating rate of 3 ℃/min under a vacuum state, keeping the temperature constant for 12 hours for pretreatment, removing water in the molten salt raw material, cooling to room temperature, taking out the molten salt, and obtaining dehydrated NaCl and dehydrated CaCl2；
(2) Preparation of the electrodes
i: 1g of MoS2Pressing the powder under 5Mpa to obtain electrode sheet with diameter of 1.6mm and thickness of 3mm, sintering, and making into MoS2The cathode is bound on the first molybdenum rod current collector by using a fine molybdenum wire;
wherein, after sintering, the molybdenum rod current collector is bound on a first molybdenum rod current collector by using a fine molybdenum wire, and the first molybdenum rod current collector is a molybdenum rod with the diameter of 1.5mm and the length of 1.2 meters.
The sintering process condition is specifically sintering for 5 hours at 850 ℃ under Ar atmosphere.
ii: polishing impurities on the surface of a graphite rod with the diameter of 10mm and the length of 100mm by 400-mesh abrasive paper, then cleaning by alcohol, drying, and fixing the graphite rod as a graphite anode on a second molybdenum rod current collector;
wherein, the second molybdenum rod current collector is a molybdenum rod with the diameter of 1.5mm and the length of 1.2 meters;
the fixing method for fixing the second molybdenum rod current collector is to drill a hole with the diameter of 1.5mm and the depth of 10mm at one end of the graphite rod and insert the molybdenum rod into the hole for fixing.
Step 2: assembling reaction system
(1) Repeatedly cleaning the stainless steel reactor with clean water, naturally drying, placing the stainless steel reactor in a muffle furnace, heating to 100 ℃, keeping the temperature for 30min at a heating rate of 3 ℃/min, cleaning and drying to obtain a dried stainless steel reactor;
(2) 163g of dehydrated NaCl and 337g of dehydrated CaCl2Putting the mixed salt into a corundum crucible, and sealing the corundum crucible in a dried stainless steel reactor;
(3) placing the sealed stainless steel reactor in a muffle furnace, heating to 300 ℃ at a heating rate of 5 ℃/min for 4h in a vacuum state, introducing argon as a protective gas, and continuously heating to 550 ℃ to obtain a molten salt system in a molten state; wherein, argon is introduced as protective gas, and the flow rate of the argon is 100 mL/min.
(4) Graphite anode and MoS2Inserting cathode into molten salt system, applying constant current of 100mA at a position 1cm away from the bottom of crucible, maintaining for 1 hr, stopping electrolysis, and adding MoS2The cathode extracts the molten salt to the upper part for cooling, and then the reactor is taken out to obtain the electrolyzed MoS2A cathode;
and step 3: post-treatment
(1) The electrolyzed MoS2Soaking the cathode in deionized water for 12h, and enabling the deionized water to react with MoS2Removing salt on the surface and in the cathode to obtain black MoS2Suspending liquid;
(2) mixing black MoS2Repeatedly cleaning the suspension with deionized water for three times, and then drying in vacuum to obtain two-dimensional layered MoS2A material; wherein, black MoS2Repeatedly cleaning the suspension with deionized water for three times, and centrifuging at 12000r/min for 5 min; and (3) performing vacuum drying, specifically performing vacuum drying at 60 ℃ for 12 h.
Example 2
Two-dimensional layered MoS prepared by molten salt electrochemical intercalation method2The method of the material comprises the following steps:
in this embodiment, the molten salt used is a chloride molten salt, specifically a mixture of LiCl-KCl, in mol ratio, LiCl: KCl ═ 0.592: 0.408.
step 1: pretreatment of LiCl and KCl salts
Weighing LiCl and KCl according to the proportion of molten salt raw materials, respectively grinding the LiCl and the KCl to obtain the LiCl and KCl with the particle size of 1.5mm, respectively pouring the LiCl and KCl into a beaker after grinding, and placing the beaker into a muffle furnace for sealing;
in a vacuum state, heating a muffle furnace to 300 ℃ at a heating rate of 4 ℃/min, keeping the temperature constant for 12h for pretreatment, removing water in a molten salt raw material, cooling to room temperature, taking out molten salt, and obtaining dehydrated LiCl and dehydrated KCl;
(2) preparation of the electrodes
i: 1g of MoS2Pressing the powder under 5Mpa to obtain electrode sheet with diameter of 1.6mm and thickness of 3mm, sintering, and making into MoS2A cathode is bound on a first molybdenum rod current collector with the diameter of 1.5mm and the length of 1.2 meters by a fine molybdenum wire;
and sintering at 850 ℃ for 5 hours in Ar atmosphere.
ii: polishing impurities on the surface of a graphite rod with the diameter of 10mm and the length of 100mm by using 400-mesh abrasive paper, cleaning the surface of the graphite rod by using alcohol, drying the graphite rod to serve as a graphite anode, drilling a hole with the diameter of 1.5mm and the depth of 10mm at one end of the graphite rod, and inserting a molybdenum rod with the diameter of 1.5mm and the length of 1.2m into the hole for fixing;
step 2: assembling reaction system
(1) Repeatedly cleaning the stainless steel reactor with clear water, naturally airing, placing in a muffle furnace, heating to 100 ℃, wherein the heating rate is 3 ℃/min, and keeping the temperature for 30min to obtain a cleaned and dried stainless steel reactor;
(2) putting 228.5g of dehydrated LiCl and 271.5g of dehydrated KCl mixed salt into a corundum crucible, and sealing the corundum crucible in a cleaned and dried stainless steel reactor;
(3) placing the sealed stainless steel reactor in a muffle furnace, heating to 300 ℃ at a heating rate of 5 ℃/min for 4h in a vacuum state, introducing argon as a protective gas, and continuously heating to 400 ℃ to obtain a molten salt system in a molten state; wherein, argon is introduced as protective gas, and the flow rate of the argon is 100 mL/min.
(4) Prepared graphite anode and MoS2Inserting cathode into molten salt 1cm away from crucible bottom, applying constant current of 100mA, maintaining for 1 hr, stopping electrolysis, and adding MoS2The cathode extracts the molten salt to the upper part for cooling, and then the reactor is taken out to obtain the electrolyzed MoS2A cathode;
and step 3: post-treatment
(1) The electrolyzed MoS2Soaking the cathode in deionized water for 12h, and soaking MoS in the deionized water2Removing salt on the surface and in the cathode to obtain black MoS2Suspension of turbid urineLiquid;
(2) mixing black MoS2Repeatedly cleaning the suspension with deionized water for three times, and then drying in vacuum to obtain two-dimensional layered MoS2A material; wherein, black MoS2Repeatedly cleaning the suspension with deionized water for three times, and centrifuging at 12000r/min for 5 min; and (3) performing vacuum drying, specifically performing vacuum drying at 60 ℃ for 12 h.
Example 3
Two-dimensional layered MoS prepared by molten salt electrochemical intercalation method2The method of the material comprises the following steps:
in this example, the molten salt used is a chloride molten salt, specifically MgCl2-mixture of NaCl-KCl in molar ratio, MgCl2：NaCl：KCl＝0.454：0.33：0.216。
Step 1: preparation of
(1)MgCl2Pretreatment of NaCl and KCl salts
The difference from example 1 is that:
1) in step 1, MgCl is added2Grinding NaCl and KCl;
2) in step 1, obtaining dehydrated MgCl2Dehydrated NaCl and dehydrated KCl salt.
(2) Preparation of the electrodes
The same as example 1;
step 2: assembly of the reaction System
The difference from example 1 is that:
1) in step 2 (2), 275g of dehydrated MgCl2122.75g of dehydrated NaCl and 102.25g of dehydrated KCl were placed in a corundum crucible.
2) In the step 2(3), the temperature is continuously increased to 450 ℃ after the vacuum is maintained at 200 ℃ for 4 h.
And step 3: post-treatment
The same as in example 1.
The other ways are the same.
Example 4
Two-dimensional layered MoS prepared by molten salt electrochemical intercalation method2Of materialsThe method differs from example 1 in that:
in step 2 (4), a constant current of 100mA is applied for 0.5 h.
Example 5
Two-dimensional layered MoS prepared by molten salt electrochemical intercalation method2The material was prepared in the same manner as in example 1, except that:
in step 2 (4), a constant current of 100mA was applied for 1.5 hours.
Example 6
Two-dimensional layered MoS prepared by molten salt electrochemical intercalation method2The material was prepared in the same manner as in example 2, except that:
in step 2 (4), a constant current of 100mA is applied for 0.5 h.
Example 7
Two-dimensional layered MoS prepared by molten salt electrochemical intercalation method2The material was prepared in the same manner as in example 2, except that:
in step 2 (4), a constant current of 100mA was applied for 1.5 hours.
Claims (10)
1. Two-dimensional layered MoS prepared by molten salt electrochemical intercalation method2A method of forming a material, comprising the steps of:
step 1: preparation of
(1) Pretreatment of molten salt feedstock
Weighing the molten salt raw materials according to the molten salt raw material components of a molten salt system, respectively pretreating the molten salt raw materials in a vacuum state, removing water in the molten salt raw materials, and cooling to room temperature to obtain the dehydrated molten salt raw materials;
the molten salt system is one of mixed molten salt systems of chloride;
(2) preparation of the electrodes
Mixing MoS2Pressing the powder into electrode plate, sintering, and fixing on the first molybdenum rod current collector as MoS2A cathode;
polishing, cleaning and drying the surface of the graphite rod, and fixing the graphite rod on a second molybdenum rod current collector to be used as a graphite anode;
step 2: assembling reaction system
(1) Cleaning and drying the molten salt electrochemical reactor to obtain a dried molten salt electrochemical reactor;
(2) mixing the dehydrated molten salt raw materials according to a molten salt system, adding the mixture into a crucible after mixing, and sealing the crucible in a dried molten salt electrochemical reactor;
(3) placing the sealed molten salt electrochemical reactor in a muffle furnace, heating to 200-500 ℃ in a vacuum state, preserving heat for 3-5 h, introducing Ar as protective gas, continuously heating to a temperature not lower than 50-100 ℃ of the melting temperature of a molten salt system, keeping the temperature for 0-30min, and electrolyzing;
(4) graphite anode and MoS2Inserting a cathode into a molten salt system, applying a constant current of 25-100 mA, electrolyzing for 0.5-6 h, and carrying out MoS2Taking out the cathode, and cooling to obtain the electrolyzed MoS2A cathode;
and step 3: post-treatment
The electrolyzed MoS2Cathode, soaking in deionized water to remove MoS2Dissolving the molten salt attached to the surface and the interior of the cathode to obtain black MoS2Suspending liquid;
mixing black MoS2Repeatedly centrifuging and ultrasonically washing the suspension to obtain MoS2Vacuum drying the solid product to obtain two-dimensional layered MoS2A material.
2. The molten salt electrochemical intercalation method of claim 1 for preparing two-dimensional layered MoS2The method for preparing the material is characterized in that in the step 1(1), the molten salt raw material is ground before being pretreated to obtain the molten salt raw material with the particle size of less than or equal to 2 mm.
3. The molten salt electrochemical intercalation method of claim 1 for preparing two-dimensional layered MoS2The method for preparing the material is characterized in that in the step 1(1), the molten salt system is NaCl-CaCl2Molten salt system, LiCl-KCl molten salt system, NaCl-KCl-MgCl2Molten salt system, NaCl-KCl-ZnCl2Molten salt systemOne of (1);
the NaCl-CaCl2In a molten salt system, the molar ratio of NaCl: CaCl2=0.479：0.521；
In the LiCl-KCl molten salt system, the molar ratio of LiCl: KCl = 0.592: 0.408 of;
in the NaCl-KCl molten salt system, the molar ratio of NaCl: KCl = 0.5: 0.5;
the NaCl-KCl-MgCl2In a molten salt system, the molar ratio of NaCl: KCl: MgCl2=0.33：0.216：0.454；
The NaCl-KCl-ZnCl2In a molten salt system, the molar ratio of NaCl: KCl: ZnCl2=0.2：0.2：0.6。
4. The molten salt electrochemical intercalation method of claim 1 for preparing two-dimensional layered MoS2The method for preparing the material is characterized in that in the step 1(1), the pretreatment comprises the following steps: heating to 200-350 ℃, keeping the temperature for 5-10 h, wherein the heating rate is 2-5 ℃/min.
5. The molten salt electrochemical intercalation method of claim 1 for preparing two-dimensional layered MoS2The method for preparing the material is characterized in that in the step 1 and the step 2, the pressing pressure is 4-5 MPa;
and sintering, namely sintering for 4-6 h at 800-900 ℃ in Ar atmosphere.
6. The molten salt electrochemical intercalation method of claim 1 for preparing two-dimensional layered MoS2The method for preparing the material is characterized in that in the step 2(1), the material is cleaned and dried, specifically, the material is repeatedly cleaned by water, naturally dried, and then placed in a muffle furnace to be heated to 100-120 ℃, the heating rate is 2-3 ℃/min, and the constant temperature is 20-60 min.
7. The molten salt electrochemical intercalation method of claim 1 for preparing two-dimensional layered MoS2The method for preparing the material is characterized in that in the step 2(3), the temperature is increased to 200-500 ℃, and the temperature increase rate is 3-5 ℃/min;and continuously heating to a temperature which is more than or equal to 50-100 ℃ of the melting temperature of the molten salt system, wherein the heating rate is 3-5 ℃/min.
8. The molten salt electrochemical intercalation method of claim 1 for preparing two-dimensional layered MoS2The method for preparing the material is characterized in that in the step 2(3), the melting temperature is 350-850 ℃.
9. The molten salt electrochemical intercalation method of claim 1 for preparing two-dimensional layered MoS2The method for preparing the material is characterized in that in the step 2(3), Ar is introduced as protective gas, and the flow rate of Ar is 80-150 mL/min.
10. The molten salt electrochemical intercalation method of claim 1 for preparing two-dimensional layered MoS2The method of the material is characterized in that in the step 3, the MoS is soaked2Completely soaking for 10-15 h; the centrifugation is carried out at the centrifugation rotating speed of 8000-12000 r/min for 5-10 min; and (3) carrying out vacuum drying at the drying temperature of 50-70 ℃ for 10-15 h.
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| CN108190960B (en) * | 2018-01-23 | 2020-05-08 | 福州大学 | Method for preparing monolayer molybdenum disulfide based on hot lithium insertion stripping of electrolyte solvent |
| CN108640154A (en) * | 2018-06-15 | 2018-10-12 | 西南交通大学 | A kind of molybdenum disulfide nano material and preparation method thereof |
| CN109110818A (en) * | 2018-09-26 | 2019-01-01 | 安阳工学院 | It is a kind of two dimension molybdenum disulfide, tungsten disulfide thin slice electrochemical preparation method |
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