CN105688942B - A kind of stratiform MoS2The preparation method of Ni nano composite materials - Google Patents

Abstract

The invention provides a preparation method of a layered MoS ₂ -Ni nanocomposite material, wherein molybdenum disulfide powder is added into a layered solution for a layered reaction to form a mixed solution; an oxidant is added to the mixed solution to carry out an oxidation intercalation reaction, After filtering and drying, the intercalated molybdenum disulfide powder was obtained; dissolving nickel acetylacetonate in tetrahydrofuran, adding the intercalated molybdenum disulfide powder, stirring and mixing for reaction, centrifuging, cleaning, and drying to obtain MoS ₂ -Ni mixed powder; MoS ₂ The /Ni mixed powder is mixed with the explosive agent for explosive reaction, and the explosive reaction product is taken out after cooling to room temperature, and the layered MoS ₂ ‑Ni nanocomposite material is obtained. The product prepared by the present invention is a composite nanomaterial of layered molybdenum disulfide and Ni nanoparticles with high carrier mobility, and the Ni nanoparticles are evenly attached to the single-layer molybdenum disulfide sheet, which improves its catalytic hydrogenation And lubricating properties, greatly expanding the scope of application of molybdenum disulfide.

Description

A kind of preparation method of layered MoS2-Ni nanocomposite material

technical field

The invention belongs to the technical field of molybdenum metal, relates to a molybdenum disulfide composite material, in particular to a preparation method of a layered MoS ₂ -Ni nanometer composite material.

Background technique

Graphene-like molybdenum disulfide (Graphene-like MoS 2 ) composed of single-layer or few-layer molybdenum disulfide (Graphene-like MoS ₂ ) is a new type of two-dimensional (2D) layered compound with graphene-like structure and properties. It has become an emerging research hotspot due to its physical and chemical properties. Graphene-like molybdenum disulfide is a two-dimensional crystal material with a "sandwich sandwich" layered structure composed of a hexagonal single-layer or multi-layer molybdenum disulfide. The single-layer molybdenum disulfide is composed of three atomic layers. The layer is a molybdenum atomic layer, and the upper and lower layers are sulfur atomic layers. The molybdenum atomic layer is sandwiched by two sulfur atomic layers to form a "sandwich" structure. Molybdenum atoms and sulfur atoms are covalently bonded to form a two-dimensional atomic crystal; Layer molybdenum disulfide is composed of several single-layer molybdenum disulfide, generally no more than five layers, there is weak van der Waals force between layers, and the layer distance is about 0.65nm.

As an important class of two-dimensional layered nanomaterials, single-layer or few-layer molybdenum disulfide is widely used in many fields such as lubricants, catalysis, energy storage, and composite materials due to its unique "sandwich sandwich" layered structure. Compared with the zero-energy bandgap of graphene, graphene-like molybdenum disulfide has an adjustable energy bandgap, which has a brighter prospect in the field of optoelectronic devices; compared with the three-dimensional bulk phase structure of silicon materials, graphene-like molybdenum disulfide Molybdenum sulfide has a nanoscale two-dimensional layered structure, which can be used to manufacture semiconductors or electronic chips with smaller specifications and higher energy efficiency, and will be widely used in the next generation of nanoelectronic devices and other fields.

Although layered molybdenum disulfide has good lubricating properties and photoelectric properties, its performance in catalysis and lubrication needs to be further improved. Combining molybdenum disulfide with other organic or inorganic particles and utilizing their synergistic effects is a great way to improve One of the methods of molybdenum disulfide properties.

Although layered molybdenum disulfide has good photoelectric properties, its performance in terms of catalytic activity and lubrication needs to be further improved. Using molybdenum disulfide in combination with other organic or inorganic particles and using their synergistic effects is a great way to improve the performance of disulfide disulfide. One of the methods of molybdenum properties.

Ni has excellent catalytic properties and is one of the commonly used hydrogenation catalysts. In addition, Ni also has certain lubricating properties. Studies have shown that Ni and MoS have synergistic lubrication and synergistic catalysis, and the preparation of MoS2/Ni composites by lithium ion intercalation combined with chemical synthesis is an effective way to improve the lubrication and catalytic performance of MoS2 and Ni (Ni- Application of MoS ₂ composites in catalytic hydrodesulfurization and dearomatization of raffinate, 2009, (25) 3:339-343).

Although the Ni-MoS ₂ composite material has been prepared by the above method, its preparation process is complex and consumes a lot of energy, which is not suitable for industrial production, and the n-butyllithium solution used has strong reducibility and activity, and is easy to burn and explode. The process requires complex and harsh conditions. Therefore, it is necessary to explore a simple method to prepare layered MoS ₂ /TiO ₂ nanocomposites using MoS ₂ powder as raw material.

Contents of the invention

Based on the problems existing in the prior art, the present invention proposes a method for preparing a layered MoS ₂ -Ni nanocomposite material to obtain a layered MoS ₂ -Ni nanocomposite material with nanoscale and superior performance, which solves the existing problems The preparation process of MoS ₂ -Ni composites is complicated, and it is difficult to industrialize the production, while improving the catalytic hydrogenation and lubricating properties of MoS ₂ -Ni composites.

It should be noted that the MoS ₂ in the layered MoS ₂ -Ni nanocomposite material in this application is a single-layer or few-layer MoS ₂ nanomaterial, and the said few-layer refers to 2-5 layers.

In order to solve the above-mentioned technical problems, the application adopts the following technical solutions to achieve:

A method for preparing a layered MoS ₂ -Ni nanocomposite material, the method comprising the following steps:

Step 1, adding molybdenum disulfide powder into the layered solution to carry out a layered reaction to form a mixed solution;

Step 2, adding an oxidizing agent to the mixed solution to carry out an oxidation intercalation reaction, and obtaining intercalated molybdenum disulfide powder after filtering and drying;

Step 3, dissolving nickel acetylacetonate in tetrahydrofuran, adding intercalated molybdenum disulfide powder, stirring and mixing for reaction, centrifuging, cleaning, and drying to obtain MoS ₂ -Ni mixed powder;

Step 4: Mix the MoS ₂ /Ni mixed powder with the explosive agent to carry out the explosive reaction, take out the explosive reaction product after cooling to room temperature, and obtain the layered MoS ₂ -Ni nanocomposite material.

The present invention also has the following distinguishing technical features:

The layered solution is ethanol solution of aromatic sulfide; the oxidant is potassium permanganate; and the explosive is picric acid.

The aromatic sulfide is polyphenylene sulfide or aromatic diamine monomer sulfide, and the mass concentration of the aromatic sulfide ethanol solution is 10%-60%.

In step 1, the specific process of the layering reaction is: grind the molybdenum disulfide powder to 200 mesh and sieve, add the molybdenum disulfide powder into the ethanol solution of aromatic sulfide, heat to 30-50°C and stir 3 ~ 12h, forming a mixed solution.

In step 1, the mass ratio of the molybdenum disulfide powder to the aromatic sulfide is 1:(10-40).

In step 2, the specific process of the oxidative intercalation reaction is: add potassium permanganate to the mixed solution, heat to 50-90°C and stir for 3-8 hours, filter, and dry the filter cake to obtain intercalation 2 Molybdenum sulfide powder.

In step 2, the mass ratio of the potassium permanganate to the molybdenum disulfide in the mixed solution is (0.5-3):1.

The specific process of the third step is: dissolving nickel acetylacetonate in tetrahydrofuran, adding intercalated molybdenum disulfide powder, stirring and mixing evenly, transferring the mixed solution to a polytetrafluoroethylene-lined reaction kettle, heating to 190~ React at 220°C for 4-9 hours, centrifuge, wash and dry to obtain MoS ₂ -Ni mixed powder.

In step 3, the tetrahydrofuran solution concentration of nickel acetylacetonate is 0.01-0.03 mg/L, and the mass ratio of nickel acetylacetonate to intercalated molybdenum disulfide powder is (0.3-2):1.

In step 4, the specific process of the explosive reaction is: mix the MoS ₂ -Ni mixed powder and picric acid evenly, put it into a high-pressure reactor, vacuumize the high-pressure reactor and feed argon, and heat to 350~ Explosion occurs at 600°C, and the explosive reactants are taken out after cooling to room temperature with the furnace, and the layered MoS ₂ -Ni nanocomposite material is obtained.

In step 4, the mass ratio of the MoS ₂ -Ni mixed powder to picric acid is 1: (0.5-3).

Compared with the prior art, the present invention has beneficial technical effects as follows:

(I) The present invention utilizes the thiophilic properties of aromatic sulfides to reduce the interlayer van der Waals force of molybdenum disulfide raw material powder, and performs intercalation and exfoliation in combination with explosion impact. The preparation of the layered MoS ₂ -Ni nanocomposite material by this method is simple in operation, does not require complex and cumbersome preparation devices, and not only has high preparation efficiency and large output.

(II) The product prepared by the present invention is a composite nanomaterial of layered molybdenum disulfide and Ni nanoparticles with high carrier mobility, and the Ni nanoparticles are evenly attached to the single-layer molybdenum disulfide sheet, which improves its Catalytic hydrogenation and lubricating properties greatly expand the application range of molybdenum disulfide.

(Ⅲ) The preparation of the layered MoS ₂ -Ni nanocomposite material in the present invention is simple in operation, does not require complex and cumbersome preparation devices, and is suitable for industrial production.

Description of drawings

FIG. 1 is the Raman spectrum of the layered MoS ₂ -Bi ₂ MoO ₆ nanocomposite material in Example 1.

FIG. 2 is a TEM image of the layered MoS ₂ —Bi ₂ MoO ₆ nanocomposite material in Example 1. FIG.

FIG. 3 is the Raman spectrum of the MoS ₂ -Bi ₂ MoO ₆ composite material in Comparative Example 1.

FIG. 4 is an SEM image of the MoS ₂ -Bi ₂ MoO ₆ composite material in Comparative Example 1. FIG.

The specific content of the present invention will be described in further detail below in conjunction with the accompanying drawings and embodiments.

detailed description

Comply with above-mentioned technical solution, the specific embodiment of the present invention is given below, it should be noted that the present invention is not limited to following specific embodiment, all equivalent transformations done on the basis of the technical solution of the present application all fall within the scope of protection of the present invention . The present invention will be described in further detail below in conjunction with the examples.

Example 1:

This example provides a method for preparing a layered MoS ₂ -Ni nanocomposite material, which specifically includes the following steps:

Step 1: Grind 10 g of molybdenum disulfide powder to 200 mesh and sieve it, add it to a 10% ethanol solution containing 100 g of polyphenylene sulfide, heat in a water bath to 30° C. and stir for 12 hours to obtain a mixed solution.

Step 2: Add 5g of KMnO ₄ powder to the mixture, heat it in a water bath to 50°C and stir for 8h, filter and dry the filter cake to obtain 3.5g of intercalated molybdenum disulfide powder.

Step 3: Dissolve 1g of nickel acetylacetonate in 100ml of tetrahydrofuran organic solvent, add 3.5g of intercalated molybdenum disulfide powder, stir and mix evenly, transfer the mixed solution to a polytetrafluoroethylene-lined reactor, and heat to 190°C for reaction After 9 hours, centrifuge, wash and dry to obtain 4g of MoS ₂ -Ni mixed powder.

Step 4: Take 3g of MoS ₂ -Ni mixed powder and 1.5g of picric acid and mix them evenly into a high-pressure reactor, vacuumize and inject argon, heat the reactor to 500°C to explode, and cool down to room temperature with the furnace The explosive reactant is taken out, and the layered MoS ₂ -Ni nanocomposite material is obtained.

The Raman spectrum of the layered MoS ₂ -Ni nanocomposite material prepared in this example is shown in FIG. 1 , and the high-resolution TEM picture is shown in FIG. 2 . The values of E _2g ¹ and A _g ¹ in the Raman spectrum in Figure 1 are 384.85 and 406.35 respectively, and the displacement difference is 21.5, which belongs to the few-layer structure MoS ₂ , indicating that the MoS ₂ in the sample prepared in this example is a layered material; The high _- resolution TEM images reveal the lattice fringes of MoS2 and Ni, and the Ni particles are attached to the surface of the layered MoS2 _nanosheets . Based on the accompanying drawings, it can be concluded that the sample prepared in this embodiment is a layered MoS ₂ -Ni nanocomposite material.

Example 2:

This example provides a method for preparing a layered MoS ₂ -Ni nanocomposite material, which specifically includes the following steps:

Step 1: Grind 10 g of molybdenum disulfide powder to 200 mesh and sieve it, add it to a 20% ethanol solution containing 200 g of polyphenylene sulfide, heat in a water bath to 40° C. and stir for 10 h to obtain a mixed solution.

Step 2: Add 10 g of KMnO ₄ powder to the mixture, heat it in a water bath to 60° C. and stir for 7 h, filter and dry the filter cake to obtain 3.2 g of intercalated molybdenum disulfide powder.

Step 3: Dissolve 1g of nickel acetylacetonate in 200ml of tetrahydrofuran organic solvent, add 2g of intercalated molybdenum disulfide powder, stir and mix evenly, transfer the mixed solution to a polytetrafluoroethylene-lined reactor, heat to 200°C for 8 hours , centrifuged, washed and dried to obtain 2.8g of MoS ₂ -Ni mixed powder.

Step 4: Take 2.8g of MoS ₂ -Ni mixed powder and 2.8g of picric acid and mix them evenly and put them into the autoclave, vacuumize and inject argon, heat the autoclave to 480°C to explode, and cool down to room temperature with the furnace The explosive reactant is taken out, and the layered MoS ₂ -Ni nanocomposite material is obtained.

The properties of the layered MoS ₂ -Ni nanocomposite material obtained in this example are basically the same as those in Example 1.

Example 3:

This example provides a method for preparing a layered MoS ₂ -Ni nanocomposite material, which specifically includes the following steps:

Step 1: Grind 10 g of molybdenum disulfide powder to 200 mesh and sieve it, add it to a 30% ethanol solution containing 300 g of polyphenylene sulfide, heat in a water bath to 50° C. and stir for 8 hours to obtain a mixed solution.

Step 2: Add 15g of KMnO ₄ powder to the mixture, heat it in a water bath to 70°C and stir for 6h, filter and dry the filter cake to obtain 3g of intercalated molybdenum disulfide powder.

Step 3: Dissolve 0.5g of nickel acetylacetonate in 150ml of tetrahydrofuran organic solvent, add 2g of intercalated molybdenum disulfide powder, stir and mix evenly, transfer the mixed solution to a polytetrafluoroethylene-lined reactor, and heat to 210°C for reaction 7h, after centrifugation, washing and drying, 2.2g of MoS ₂ -Ni mixed powder was obtained.

Step 4: Take 2.2g of MoS ₂ -Ni mixed powder and 3.3g of picric acid and mix them evenly into a high-pressure reactor, vacuumize and inject argon, heat the reactor to 450°C to explode, and cool down to room temperature with the furnace The explosive reactant is taken out, and the layered MoS ₂ -Ni nanocomposite material is obtained.

The properties of the layered MoS ₂ -Ni nanocomposite material obtained in this example are basically the same as those in Example 1.

Example 4:

This example provides a method for preparing a layered MoS ₂ -Ni nanocomposite material, which specifically includes the following steps:

Step 1: Take 10g of molybdenum disulfide powder and grind it to 200 mesh and sieve it, add it to an ethanol solution with a concentration of 40% and containing 400g of aromatic diamine monomer sulfide, heat it in a water bath to 35°C and stir for 7h to obtain a mixed liquid.

Step 2: Add 25g of KMnO ₄ powder to the mixture, heat it in a water bath to 80°C and stir for 5h, filter and dry the filter cake to obtain 2.8g of intercalated molybdenum disulfide powder.

Step 3: Dissolve 2g of nickel acetylacetonate in 200ml of tetrahydrofuran organic solvent, add 1g of intercalated molybdenum disulfide powder, stir and mix evenly, transfer the mixed solution to a polytetrafluoroethylene-lined reactor, heat to 220°C for 6h , centrifuged, washed and dried to obtain 2.7g of MoS ₂ -Ni mixed powder.

Step 4: Take 2.7g of MoS ₂ -Ni mixed powder and 5.4g of picric acid and mix them evenly into a high-pressure reactor, vacuumize and inject argon, heat the reactor to 550°C to explode, and cool down to room temperature with the furnace The explosive reactant is taken out, and the layered MoS ₂ -Ni nanocomposite material is obtained.

The properties of the layered MoS ₂ -Ni nanocomposite material obtained in this example are basically the same as those in Example 1.

Example 5:

This example provides a method for preparing a layered MoS ₂ -Ni nanocomposite material, which specifically includes the following steps:

Step 1: Take 10g of molybdenum disulfide powder and grind it to 200 mesh and sieve it, add it to an ethanol solution with a concentration of 60% and containing 300g of aromatic diamine monomer sulfide, heat it in a water bath to 45°C and stir for 5h to obtain a mixed liquid.

Step 2: Add 20g of KMnO ₄ powder into the mixture, heat it in a water bath to 85°C and stir for 4h, filter and dry the filter cake to obtain 2.6g of intercalated molybdenum disulfide powder.

Step 3: Dissolve 2g of nickel acetylacetonate in 250ml of tetrahydrofuran organic solvent, add 2g of intercalated molybdenum disulfide powder, stir and mix evenly, transfer the mixed solution to a polytetrafluoroethylene-lined reactor, heat to 210°C for 8 hours , centrifuged, washed and dried to obtain 3.5g MoS ₂ -Ni mixed powder.

Step 4: Take 3g of MoS ₂ -Ni mixed powder and 7.5g of picric acid and mix them evenly into a high-pressure reactor, vacuumize and inject argon, heat the reactor to 510°C to explode, and take it out after cooling to room temperature with the furnace Explosive reactants, that is, layered MoS ₂ -Ni nanocomposites are obtained.

The properties of the layered MoS ₂ -Ni nanocomposite material obtained in this example are basically the same as those in Example 1.

Embodiment 6:

This example provides a method for preparing a layered MoS ₂ -Ni nanocomposite material, which specifically includes the following steps:

Step 1: Take 10g of molybdenum disulfide powder and grind it to 200 mesh and sieve it, add it to an ethanol solution with a concentration of 50% and containing 200g of aromatic diamine monomer sulfide, heat it in a water bath to 50°C and stir for 3h to obtain a mixed liquid.

Step 2: Add 10 g of KMnO ₄ powder to the mixture, heat it in a water bath to 90° C. and stir for 3 h, filter and dry the filter cake to obtain 3 g of intercalated molybdenum disulfide powder.

Step 3: Dissolve 1.5g of nickel acetylacetonate in 150ml of tetrahydrofuran organic solvent, add 2g of intercalated molybdenum disulfide powder, stir and mix evenly, transfer the mixed solution to a polytetrafluoroethylene-lined reactor, and heat to 190°C for reaction 7h, after centrifugation, washing and drying, 3.2g of MoS ₂ -Ni mixed powder was obtained.

Step 4: Take 3g of MoS ₂ -Ni mixed powder and 9g of picric acid and mix them evenly into a high-pressure reactor, vacuumize and inject argon, heat the reactor to 500°C to explode, and take it out after cooling to room temperature with the furnace. The reactant, that is, the layered MoS ₂ -Ni nanocomposite material is obtained.

The properties of the layered MoS ₂ -Ni nanocomposite material obtained in this example are basically the same as those in Example 1.

Comparative example 1:

This example provides a method for preparing a MoS ₂ -Ni composite material, which specifically includes the following steps:

Step 1: Take 10g of molybdenum disulfide powder and grind it to 200 mesh and sieve it, add it to an ethanol solution with a concentration of 5% and containing 50g of aromatic diamine monomer sulfide, heat it in a water bath to 25°C and stir for 2h to obtain a mixed liquid.

Step 2: Add 5g of KMnO ₄ powder into the mixture, heat it in a water bath to 45°C and stir for 9h, filter and dry the filter cake to obtain 3.2g of molybdenum disulfide pretreated powder.

Step 3: Dissolve 2g of nickel acetylacetonate in 100ml of tetrahydrofuran organic solvent, add 3g of intercalated molybdenum disulfide powder, stir and mix evenly, transfer the mixed solution to a polytetrafluoroethylene-lined reactor, heat to 230°C for 5 hours , centrifuged, washed and dried to obtain 4.5g MoS ₂ -Ni mixed powder.

Step 4: Take 3g of MoS ₂ -Ni mixed powder and 1g of picric acid and mix them evenly into a high-pressure reactor, vacuumize and inject argon, heat the reactor to 600°C to explode, and take it out after cooling to room temperature with the furnace. reactant, to obtain MoS ₂ -Ni composite.

Raman spectrum analysis and TEM analysis were performed on the MoS ₂ -Ni composite prepared in this comparative example.

The Raman spectrum is shown in Figure 3. The values of E _2g ¹ and A _g ¹ are 383.52 and 408.58 respectively, and the displacement difference is 25.06, which belongs to the block structure MoS ₂ .

The SEM image is shown in Figure 4, indicating that the product MoS ₂ is bulky and multilayered, and no obvious Ni particles are found on or around the MoS ₂ surface, which does not belong to single-layer or few-layer molybdenum disulfide nanocomposites.

Comparative example 2:

This example provides a method for preparing a MoS ₂ -Ni composite material, which specifically includes the following steps:

Step 1: Take 10g of molybdenum disulfide powder and grind it to 200 mesh and sieve it, add it to an ethanol solution with a concentration of 70% and containing 500g of aromatic diamine monomer sulfide, heat it in a water bath to 60°C and stir for 4h to obtain a mixed liquid.

Step 2: Add 2g of KMnO ₄ powder into the mixture, heat it in a water bath to 35°C and stir for 2h, filter and dry the filter cake to obtain 2.8g of molybdenum disulfide pretreated powder.

Step 3: Dissolve 1g of nickel acetylacetonate in 250ml of tetrahydrofuran organic solvent, add 2.5g of intercalated molybdenum disulfide powder, stir and mix evenly, transfer the mixed solution to a polytetrafluoroethylene-lined reactor, and heat to 180°C for reaction After 6 hours, centrifuge, wash and dry to obtain 3.2g of MoS ₂ -Ni mixed powder.

Step 4: Take 3g of MoS ₂ -Ni mixed powder and 1.5g of picric acid and mix them evenly into the autoclave, vacuumize and inject argon, heat the autoclave to 650°C to explode, and take it out after cooling to room temperature with the furnace Explode the reactant to get MoS ₂ -Ni composite.

The MoS ₂ -Ni composite material prepared in this comparative example is the same as the comparative example 1, and the bulk accumulation, and Ni particles appear on the surface and surrounding of the MoS ₂ bulk, which does not belong to single-layer or few-layer molybdenum disulfide nanocomposites.

Comparative example 3:

This example provides a method for preparing a MoS ₂ -Ni composite material, which specifically includes the following steps:

Step 1: Take 10g of molybdenum disulfide powder and grind it to 200 mesh and sieve it, add it to an ethanol solution with a concentration of 8% and containing 60g of aromatic diamine monomer sulfide, heat it in a water bath to 70°C and stir for 6h to obtain a mixed liquid.

Step 2: Add 25g of KMnO ₄ powder into the mixture, heat it in a water bath to 20°C and stir for 10h, filter and dry the filter cake to obtain 3.5g of molybdenum disulfide pretreated powder.

Step 3: Dissolve 3.5g of nickel acetylacetonate in 100ml of tetrahydrofuran organic solvent, add 1g of intercalated molybdenum disulfide powder, stir and mix evenly, transfer the mixed solution to a polytetrafluoroethylene-lined reactor, and heat to 240°C for reaction After 7 hours, centrifuge, wash and dry to obtain 4.3g of MoS ₂ -Ni mixed powder.

Step 4: Take 3g of MoS ₂ -Ni mixed powder and 10g of picric acid and mix them evenly into a high-pressure reactor, vacuumize and inject argon, heat the reactor to 620°C to explode, and take it out after cooling to room temperature with the furnace. reactant, to obtain MoS ₂ -Ni composite.

The MoS ₂ -Ni composite material prepared in this comparative example is the same as the comparative example 1, and the bulk accumulation, and Ni particles appear on the surface and surrounding of the MoS ₂ bulk, which does not belong to single-layer or few-layer molybdenum disulfide nanocomposites.

Claims (5)

1. A kind of 1. stratiform MoS₂The preparation method of-Ni nano composite materials, it is characterised in that：This method comprises the following steps：

   Step 1, molybdenum disulfide powder is added in layering solution and carries out layering reaction, forms mixed liquor；

   Described layering solution is the ethanol solution of aromatic thioether；

   Described aromatic thioether is polyphenylene sulfide or aromatic diamine monomer thioether, the quality of the ethanol solution of aromatic thioether Concentration is 10%~60%；

   The detailed process of described layering reaction is：Molybdenum disulfide powder is ground to the sieving of 200 mesh, by molybdenum disulfide powder plus In the ethanol solution for entering aromatic thioether, it is heated to 30~50 DEG C and stirs 3~12h, form mixed liquor；

   Step 2, addition oxidant carries out oxidation intercalation in mixed liquor, and intercalation molybdenum disulphide powder is obtained after filtration drying End；

   Described oxidant is potassium permanganate；

   The detailed process of described oxidation intercalation is：Potassium permanganate is added into mixed liquor, 50~90 DEG C is heated to and stirs 3~8h is mixed, filters, filter cake is dried, obtains intercalation molybdenum disulfide powder；

   Step 3, nickel acetylacetonate is dissolved in tetrahydrofuran, adds intercalation molybdenum disulfide powder, be stirred and reacted, Centrifugation, cleaning, obtain MoS after drying₂- Ni mixed-powders；

   The detailed process of described step three is：Nickel acetylacetonate is dissolved in tetrahydrofuran, adds intercalation molybdenum disulfide powder, Mixed liquor is transferred in polytetrafluoroethyllining lining reactor after being uniformly mixed, is heated to 190~220 DEG C of 4~9h of reaction, Centrifugation, cleaning, obtain MoS after drying₂- Ni mixed-powders；

   Step 4, by MoS₂/ Ni mixed-powders mix with burster, carry out explosive reaction, explosive reaction is taken out after being cooled to room temperature Product, that is, obtain stratiform MoS₂- Ni nano composite materials；

   Described burster is picric acid；

   The detailed process of described explosive reaction is：By MoS₂- Ni mixed-powders are well mixed with picric acid, load reaction under high pressure In kettle, autoclave is vacuumized and is passed through argon gas, be heated to 350~600 DEG C and explode, taken after cooling to room temperature with the furnace Go out explosive reaction thing, that is, obtain stratiform MoS₂- Ni nano composite materials.
2. 2. preparation method as claimed in claim 1, it is characterised in that：In step 1, described molybdenum disulfide powder and fragrance The mass ratio of race's thioether is 1:(10~40).
3. 3. preparation method as claimed in claim 1, it is characterised in that：In step 2, in described potassium permanganate and mixed liquor The mass ratio of molybdenum disulfide be (0.5~3):1.
4. 4. preparation method as claimed in claim 1, it is characterised in that：It is described in step 3：The tetrahydrochysene furan of nickel acetylacetonate Solution concentration of muttering is 0.01~0.03mg/L, the mass ratio of described nickel acetylacetonate and intercalation molybdenum disulfide powder for (0.3~ 2):1。
5. 5. preparation method as claimed in claim 1, it is characterised in that：In step 4, described MoS₂- Ni mixed-powders and hardship Sour mass ratio 1：(0.5~3).