CN104900867B - Preparation method of CNT/Co/MoS2 composite material - Google Patents

Abstract

_A preparation method of a CNT/Co/MoS2 composite material, which relates to a modification method of _MoS2 . The purpose of the present invention is to solve the problem that existing molybdenum sulfide surface modification treatment methods have modified MoS ₂ still has hydrophobicity, or the surface modification treatment method involves a large amount of organic solvents, causing serious environmental pollution problems. Preparation methods: 1. acid treatment to obtain acidified carbon nanotubes; 2. preparation of CNT/Co; 3. loading MoS ₂ to obtain CNT/Co/MoS ₂ composite material. Advantages: The coating of MoS ₂ on the surface of carbon nanotubes is relatively uniform. _The invention is mainly used for preparing CNT/Co/MoS2 composite material.

Description

A kind of preparation method of CNT/Co/MoS2 composite material

technical field

_The invention relates to a method for modifying MoS2.

Background technique

China is rich in molybdenite resources. Molybdenite (MoS ₂ ) has many excellent properties, such as lubrication, catalysis, energy storage and photoelectric properties, which are favored by the scientific and industrial circles. Especially for catalytic performance, compared with traditional catalysts, MoS2 not only has high catalytic efficiency, but also can effectively avoid _hydrogen sulfide poisoning that often occurs in the catalytic process of noble metals such as Pt. However, in most applications of MoS ₂ , such as catalysis and energy storage, molybdenite is insoluble in water, which directly limits the application of MoS ₂ . At present, the solution to this problem mainly depends on: 1) the resynthesis of molybdate and sulfur source; ₂ ) the surface modification of MoS2 by surfactants with the participation of organic solvents. Relying on the resynthesis method of molybdenum sulfide with molybdate and sulfur source, although MoS ₂ with high catalytic activity can be obtained, the MoS ₂ with high catalytic activity still has the problem of hydrophobicity; the second surface modification The permanent treatment method will cause serious environmental pollution problems because it involves a large amount of organic solvents, and it is also difficult to produce in batches.

Contents of the invention

_The purpose of the present invention is to solve the problem that the modified _MoS still has hydrophobicity in the existing MoS2 surface modification treatment method, or the surface modification treatment method involves a large amount of organic solvents, causing serious environmental pollution problems, A method for preparing a CNT/Co/MoS ₂ composite material is provided.

A kind of preparation method of CNT/Co/MoS ₂ composite material, specifically is finished according to the following steps: 1, acid treatment: put carbon nanotube into acid and carry out acid treatment, obtain the carbon nanotube after acidification; 2, prepare CNT /Co: The acidified carbon nanotubes are uniformly dispersed in distilled water with the assistance of ultrasonic waves to obtain a carbon nanotube dispersion, and then cobalt nitrate is dissolved in the carbon nanotube dispersion under ultrasonic conditions to obtain a cobalt-containing carbon nanotube mixture , adding an aqueous solution of sodium borohydride dropwise to the cobalt-containing carbon nanotube mixture in an ultrasonic state, and then filtering, using deionized water to rinse the solid-phase filtrate for 2 to 4 times to obtain the cleaned solid-phase filtrate, Carry out vacuum drying to the solid phase filtrate after cleaning again, obtain CNT/Co; The mass fraction of carbon nanotubes after acidification in the carbon nanotube dispersion liquid described in step 2 is 0.1%～1%; Described in step 2 The mass fraction of cobalt nitrate in the cobalt-containing carbon nanotube mixture is 0.3%～3%; the volume ratio of the sodium borohydride aqueous solution and distilled water described in step 2 is (0.8～1.2):10, and the sodium borohydride The mass fraction of sodium borohydride in the aqueous solution is 2% to 30%; 3. Loading MoS ₂ : uniformly disperse CNT/Co in distilled water with the assistance of ultrasonic waves to obtain a CNT/Co dispersion, and then add MoS ₂ Add CNT/Co dispersion liquid to the powder, and continue to ultrasonically disperse for 2h~5h to obtain a mixture, let it stand for stratification, take the lower layer and filter to obtain a solid phase, rinse the solid phase with deionized water, and rinse until the filter Until the surface of the liquid has no metallic luster, the solid phase after cleaning is obtained, and then the solid phase after cleaning is vacuum-dried to obtain a CNT/Co/MoS ₂ composite material. In the CNT/Co dispersion described in step 3, CNT/ The mass fraction of Co is 0.1%-1%, and the mass fraction of MoS ₂ powder in the mixture described in step 3 is 0.2%-3%.

Advantages of the present invention: _1. In the method for preparing CNT/Co/MoS2 composite materials in the present invention, commercially available _MoS2 powder is directly used as the preparation raw material, and the reaction process is a preparation process at normal temperature and pressure, and the required reaction equipment is also simple and the cost is low. Low; two, the present invention adopts the magnetic synthesis method, and the MoS coating _on the carbon nanotube surface is relatively uniform; three, the present invention prepares CNT/Co/MoS _The method for the composite material is suitable for large-scale synthesis; four, the present invention prepares _The CNT/Co/MoS2 composites have a wide range of applications in catalysts, solar cells, Li-ion batteries, sensors, etc.

Description of drawings

Fig. 1 is the CNT/Co isothermal hysteresis loop diagram that test one step two obtains;

Fig. ₂ is the isothermal hysteresis loop diagram of the CNT/Co/MoS composite material obtained in the first test;

Fig. 3 is the cyclic voltammogram of CNT/Co working electrode;

Figure ₄ is the cyclic voltammetry spectrum of the CNT/Co/MoS2 working electrode;

Fig. 5 is the CNT/Co Raman spectrogram that test one step two obtains;

Figure 6 is the Raman spectrum of the CNT/Co/MoS composite obtained in Experiment ₁ ;

Figure 7 is the It response curve of CNT/Co/MoS ₂ working electrode to H ₂ S alkaline solution;

Fig. 8 is the CNT/Co scanning electron micrograph obtained in the second step of the second test;

Figure 9 is a scanning electron micrograph of the CNT/Co/MoS composite material prepared in this experiment _;

Fig. 10 is the CNT/Co transmission electron microscope image obtained in the second step of the second test;

Figure 11 is a transmission electron microscope image of the CNT/Co/MoS ₂ composite material prepared in this experiment.

detailed description

Specific embodiment 1: This embodiment is a preparation method of CNT/Co/MoS ₂ composite material, which is completed according to the following steps: 1. Acid treatment: put carbon nanotubes into acid for acid treatment to obtain acidified Second, preparation of CNT/Co: uniformly disperse the acidified carbon nanotubes into distilled water under the assistance of ultrasonic waves to obtain a carbon nanotube dispersion, and then dissolve cobalt nitrate in the carbon nanotube dispersion under ultrasonic conditions , to obtain a cobalt-containing carbon nanotube mixture, add an aqueous solution of sodium borohydride dropwise to the cobalt-containing carbon nanotube mixture in an ultrasonic state, then filter, and use deionized water to rinse the solid-phase filtrate for 2 to 4 times , to obtain the solid-phase filtrate after cleaning, and then vacuum-dry the solid-phase filtrate after cleaning to obtain CNT/Co; the mass fraction of carbon nanotubes after acidification in the carbon nanotube dispersion described in step 2 is 0.1%～ 1%; The massfraction of cobalt nitrate in the cobalt-containing carbon nanotube mixture described in step 2 is 0.3%～3%; The volume ratio of sodium borohydride aqueous solution and distilled water described in step 2 is (0.8～1.2): 10, and the mass fraction of sodium borohydride in the sodium borohydride aqueous solution is 2% to 30%; 3. Loading MoS ₂ : uniformly disperse CNT/Co in distilled water under the assistance of ultrasonic waves to obtain a CNT/Co dispersion , and then add MoS ₂ powder into CNT/Co dispersion liquid under ultrasonic state, and continue ultrasonic dispersion for 2h~5h to obtain the mixture, stand to separate layers, take the lower layer liquid and filter to obtain solid phase, use deionized water to The solid phase is washed until the surface of the filtrate has no metallic luster, and the cleaned solid phase is obtained, and then the cleaned solid phase is vacuum-dried to obtain a CNT/Co/MoS ₂ composite material, as described in step 3 The mass fraction of CNT/Co in the CNT/Co dispersion liquid is 0.1%-1%, and the mass fraction of MoS ₂ powder in the mixture described in step 3 is 0.2%-3%.

Specific embodiment two: the difference between this embodiment and specific embodiment one is: the acid described in step one is concentrated nitric acid-concentrated sulfuric acid mixed acid, the volume ratio of described concentrated nitric acid and concentrated sulfuric acid is 1:3, the described The mass fraction of the concentrated nitric acid is 60%-68%, and the mass fraction of the concentrated sulfuric acid is 68%-75%. Others are the same as the first embodiment.

Specific embodiment three: the difference between this embodiment and specific embodiment one or two is: the acid treatment described in step 1 is specifically operated as follows: carbon nanotubes are put into concentrated nitric acid-concentrated sulfuric acid mixed acid, at a temperature of The acid treatment was completed by ultrasonic treatment at 50°C for 6 hours, and the volume ratio of the mass of the carbon nanotubes to the mixed acid of concentrated nitric acid-concentrated sulfuric acid was 1g:40mL. Others are the same as those in Embodiment 1 or 2.

Embodiment 4: This embodiment differs from Embodiment 1 to Embodiment 3 in that: the specific operation of the vacuum drying described in step 2 is as follows: vacuum drying at a temperature of 70° C. for 6 hours. Others are the same as the specific embodiments 1 to 3.

Embodiment 5: This embodiment differs from Embodiments 1 to 4 in that the mass fraction of carbon nanotubes in the carbon nanotube dispersion described in step 2 after acidification is 0.1% to 0.5%. Others are the same as the specific embodiments 1 to 4.

Embodiment 6: This embodiment differs from Embodiment 1 to Embodiment 5 in that the mass fraction of cobalt nitrate in the cobalt-containing carbon nanotube mixture described in step 2 is 0.6% to 1.5%. Others are the same as the specific embodiments 1 to 5.

Specific embodiment seven: the difference between this embodiment and one of specific embodiments one to six is: the volume ratio of the sodium borohydride aqueous solution and distilled water described in step 2 is 1:10, and the boron in the described sodium borohydride aqueous solution The mass fraction of sodium hydride is 2% to 10%. Others are the same as the specific embodiments 1 to 6.

Embodiment 8: This embodiment differs from Embodiment 1 to Embodiment 7 in that: the specific operation of the vacuum drying described in Step 3 is as follows: vacuum drying at a temperature of 70° C. for 6 hours. Others are the same as those in Embodiments 1 to 7.

Embodiment 9: This embodiment differs from Embodiments 1 to 8 in that the mass fraction of CNT/Co in the CNT/Co dispersion described in Step 3 is 0.1%-0.5%. Others are the same as the specific embodiments 1 to 8.

Embodiment 10: The difference between this embodiment and Embodiment 1 to Embodiment 9 is that the mass fraction of MoS ₂ powder in the mixture described in Step 3 is 0.2%-1%. Others are the same as the specific embodiments 1 to 9.

Adopt following test verification effect of the present invention

Test 1: A preparation method of CNT/Co/MoS ₂ composite material, which is completed according to the following steps: 1. Acid treatment: put carbon nanotubes into acid for acid treatment to obtain acidified carbon nanotubes; 2. 1. Preparation of CNT/Co: Disperse acidified carbon nanotubes evenly in distilled water under the assistance of ultrasonic waves to obtain a carbon nanotube dispersion, and then dissolve 600 mg of cobalt nitrate in 100 mL of carbon nanotube dispersion under ultrasonic conditions to obtain a carbon nanotube dispersion containing For the cobalt-carbon nanotube mixture, 10 mL of sodium borohydride solution with a mass fraction of 5% was added dropwise to the cobalt-containing carbon nanotube mixture in an ultrasonic state, and then filtered, and the solid-phase filtrate was rinsed with deionized water for 3 second, obtain the solid phase filtrate after cleaning, then vacuum-dry the solid phase filtrate after cleaning to obtain CNT/Co; the mass fraction of carbon nanotubes after acidification in the carbon nanotube dispersion described in step 2 is 0.1% ; 3. Loading MoS ₂ : uniformly disperse CNT/Co into distilled water with the assistance of ultrasonic waves to obtain a CNT/Co dispersion, then add MoS ₂ powder to the CNT/Co dispersion under ultrasonic conditions, and continue ultrasonic dispersion for 2 hours , to obtain the mixture, leave it to stand for stratification, remove the lower layer of liquid and filter to obtain a solid phase, use deionized water to wash the solid phase until the surface of the filtrate has no metallic luster, and obtain the solid phase after cleaning, and then Carry out vacuum drying to the solid phase after cleaning, obtain CNT/Co/MoS Composite material, the mass fraction of CNT/Co in the CNT/Co dispersion liquid described in step ₃ is 0.1%, in the mixture described in step 3 The mass fraction of MoS ₂ powder is 0.2%.

The acid described in this test step one is concentrated nitric acid-concentrated sulfuric acid mixed acid, the volume ratio of described concentrated nitric acid and concentrated sulfuric acid is 1:3, the mass fraction of described concentrated nitric acid is 65%, the mass fraction of described concentrated sulfuric acid 70%.

The specific operation of the acid treatment described in step 1 of this test is as follows: put the carbon nanotubes into concentrated nitric acid-concentrated sulfuric acid mixed acid, and ultrasonically treat them for 6 hours at a temperature of 50°C to complete the acid treatment. The volume ratio of mass to concentrated nitric acid-concentrated sulfuric acid mixed acid is 1g:40mL.

The specific operation of the vacuum drying described in the second step of the test is as follows: vacuum drying at a temperature of 70° C. for 6 hours.

The specific operation of the vacuum drying described in the third step of the test is as follows: vacuum drying at a temperature of 70° C. for 6 hours.

The CNT/Co obtained in step 2 of this test and the CNT/Co/MoS ₂ composite material obtained in this test were tested for magnetic properties. The test results are shown in Figure 1 and Figure 2. Figure 1 is the CNT/Co isothermal obtained in step 2 of test 1. Hysteresis loop diagram; Figure ₂ is the isothermal hysteresis loop diagram of the CNT/Co/MoS composite material obtained in the first test; as can be seen from Figure 1 and Figure 2, the CNT/Co obtained in the second test step and this test The obtained CNT/Co/MoS ₂ composites are all ferromagnetic substances with magnetic saturation phenomenon. When MoS ₂ is loaded on the outer layer of CNT/Co, the magnetic properties of the material are enhanced and the magnetic moment increases, indicating that MoS ₂ in the CNT/Co/MoS ₂ composite obtained in this experiment has ferromagnetism.

The CNT/Co obtained in this test step ₂ and the CNT/Co/MoS composite material obtained in this test are electrochemically tested, and the specific methods are as follows:

Disperse 2 mg of the CNT/Co obtained in step 2 of this test in 10 mL of 0.5% (V/W) Nafion-ethanol solution to obtain a dispersion, and then apply the dispersion onto the surface of a clean glassy carbon electrode (the glassy carbon electrodes are successively passed through Polishing and cleaning to obtain a clean glassy carbon electrode), and natural drying to obtain a CNT/Co working electrode.

Disperse _2mg of the CNT/Co/MoS2 composite material obtained in this test in 10mL of 0.5% (V/W) Nafion-ethanol solution to obtain a dispersion, and then apply the dispersion to the surface of a clean glassy carbon electrode (glassy carbon The electrode was polished and cleaned in turn to obtain a clean glassy carbon electrode), and after natural drying, a CNT/Co/MoS ₂ working electrode was obtained.

The CNT/Co working electrode and the CNT/Co/MoS ₂ working electrode were respectively used as the working electrodes, and the electrochemical test was carried out in the NaH ₂ PO ₄ /Na ₂ HPO ₄ buffer solution with pH = 7.0, the sweep rate: 50mV/s, the test The results are shown in Figure 3 and Figure 4, Figure 3 is the cyclic voltammetry spectrum of the CNT/Co working electrode; Figure 4 is the cyclic voltammetry spectrum of the CNT/Co/MoS ₂ working electrode; by Figure 3 and Figure 4 it can be known , the characteristic peak shape and position of the cyclic voltammetry spectrum of the CNT/Co/MoS ₂ working electrode are not the result of superposition on the basis of the cyclic voltammetry spectrum of the CNT/Co working electrode, but the shift of the peak (0.5V and 1.5V) and a new peak (about -1.8V), indicating that MoS ₂ is not only successfully supported on the CNT/Co substrate, but also MoS ₂ and CNT/Co substrate have a synergistic interaction.

The CNT/Co obtained in step ₂ of this test and the CNT/Co/MoS composite material obtained in this test were analyzed by Raman spectroscopy. The test results are shown in Figure 5 and Figure 6, and Figure 5 is the CNT/Co obtained in step 2 of test 1. Co Raman spectrum; Figure 6 is the Raman spectrum of the CNT/Co/MoS ₂ composite material obtained in Experiment 1; through the analysis of the spectrum results in Figure 5 and Figure 6, it can be known that carbon nanotubes are near 1326cm ^-1 and 1575cm ^-1 The characteristic peaks D and G of MoS ₂ . The peaks around 369cm ^-1 and 408cm ^-1 are the characteristic peaks of E _2g ¹ and A _1g of MoS ₂ . Compared with the standard Raman spectrum of MoS 2 , it is found that the position of the E _2g ¹ peak appears blue The position of the characteristic peak of A _1g shifted red shifted, indicating that the layered structure of MoS ₂ in the CNT/Co/MoS ₂ composite material changed from a multi-layer structure to a single-layer or few-layer structure, that is, lamellar MoS ₂ Peeling occurs. The exfoliation of MoS ₂ causes the generation or appearance of flake MoS ₂ edge defects, which is the fundamental reason for the ferromagnetism of MoS ₂ in the CNT/Co/MoS ₂ composite obtained in this experiment.

Experiment 2: A preparation method of a CNT/Co/MoS ₂ composite material, which is completed according to the following steps: 1. Acid treatment: put carbon nanotubes into acid for acid treatment to obtain acidified carbon nanotubes; 2. 1. Preparation of CNT/Co: Disperse acidified carbon nanotubes evenly in distilled water under the assistance of ultrasonic waves to obtain a carbon nanotube dispersion, and then dissolve 1500 mg of cobalt nitrate in 100 mL of a carbon nanotube dispersion under ultrasonic conditions to obtain a carbon nanotube dispersion containing For the cobalt-carbon nanotube mixture, 10 mL of sodium borohydride solution with a mass fraction of 5% was added dropwise to the cobalt-containing carbon nanotube mixture in an ultrasonic state, and then filtered, and the solid-phase filtrate was rinsed with deionized water for 3 second, obtain the solid-phase filtrate after cleaning, then vacuum-dry the solid-phase filtrate after cleaning to obtain CNT/Co; the massfraction of carbon nanotubes after acidification in the carbon nanotube dispersion described in step 2 is 0.5% ; 3. Loading MoS ₂ : uniformly disperse CNT/Co into distilled water with the assistance of ultrasonic waves to obtain a CNT/Co dispersion, then add MoS ₂ powder to the CNT/Co dispersion under ultrasonic conditions, and continue ultrasonic dispersion for 2 hours , to obtain the mixture, leave it to stand for stratification, remove the lower layer of liquid and filter to obtain a solid phase, use deionized water to wash the solid phase until the surface of the filtrate has no metallic luster, and obtain the solid phase after cleaning, and then Carry out vacuum drying to the solid phase after cleaning, obtain CNT/Co/MoS ₂ Composite material, the mass fraction of CNT/Co in the CNT/Co dispersion described in step 3 is 0.2%, in the mixture described in step 3 The mass fraction of MoS ₂ powder is 0.5%.

The acid described in this test step one is concentrated nitric acid-concentrated sulfuric acid mixed acid, the volume ratio of described concentrated nitric acid and concentrated sulfuric acid is 1:3, the mass fraction of described concentrated nitric acid is 65%, the mass fraction of described concentrated sulfuric acid 70%.

The specific operation of the acid treatment described in step 1 of this test is as follows: put the carbon nanotubes into concentrated nitric acid-concentrated sulfuric acid mixed acid, and ultrasonically treat them for 6 hours at a temperature of 50°C to complete the acid treatment. The volume ratio of mass to concentrated nitric acid-concentrated sulfuric acid mixed acid is 1g:40mL.

The specific operation of the vacuum drying described in the second step of the test is as follows: vacuum drying at a temperature of 70° C. for 6 hours.

The specific operation of the vacuum drying described in the third step of the test is as follows: vacuum drying at a temperature of 70° C. for 6 hours.

Detect the It response curve of the CNT/Co/MoS ₂ composite material prepared in this test to H ₂ S alkaline solution, the specific process is as follows:

Disperse 2 mg of the CNT/Co/MoS ₂ composite material obtained in this test in 10 mL of 0.05% (V/W) Nafion-ethanol solution to obtain a dispersion, and then apply 15 μL of the dispersion to the surface of a polished glassy carbon electrode (glass The carbon electrode was sequentially polished with 0.3 μm α-Al ₂ O ₃ powder and 0.05 μm α-Al ₂ O ₃ powder to obtain a polished glassy carbon electrode), and after natural drying, a CNT/Co/MoS ₂ working electrode was obtained.

Using the CNT/Co/MoS ₂ working electrode as the working electrode, put the CNT/Co/MoS ₂ working electrode into the H ₂ S alkaline solution (the H ₂ S alkaline solution is made by mixing H ₂ S, NaOH and deionized water , pH is 7.3), with the platinum electrode as the counter electrode and the calomel electrode as the auxiliary electrode, the current-time test is carried out. After the test was performed for 50 seconds, 75 μL of H ₂ S alkaline solution was added every 20 seconds. The test results are shown in Figure 7. Figure 7 is the It response curve of the CNT/Co/MoS ₂ working electrode to the H ₂ S alkaline solution; it can be seen from Figure 7 that the CNT/Co/MoS ₂ working electrode is exposed to an applied voltage of 0.5V Around, with the increasing amount of H ₂ S alkaline solution, the current increment is increasing, and the stable current value is also increasing, the response time is about 0.2 seconds, which shows that the CNT/Co/MoS ₂ working electrode performance The obvious H ₂ S sensitive performance is shown, which proves that the CNT/Co/MoS ₂ composite prepared in this experiment can be applied in H ₂ S or Na ₂ S sensing devices.

Figure 8 is the SEM image of CNT/Co obtained in Step 2 of Test 2; Figure 9 is the SEM image of the CNT/Co/MoS ₂ composite material prepared in this test; Figure 10 is the TEM image of CNT/Co obtained in Step 2 of Test 2 ; Fig. 11 is the CNT/Co/ _{MoS2composite} material transmission electron microscope image prepared in this test; It can be known from Fig. 8-11 that the CNT/Co obtained in the second step of the test and the CNT/Co/ _{MoS2composite} material prepared in this test _The thickness of the nanotube wall in the TEM image is uniform, indicating that Co and MoS ₂ are evenly distributed _on the surface of the CNT. on the CNT substrate.

Claims (10)

1. a kind of CNT/Co/MoS₂The preparation method of composite, it is characterised in that CNT/Co/MoS₂The preparation side of composite Method is completed according to the following steps：First, acid treatment：CNT is put in acid carries out acid treatment, carbon nanometer after being acidified Pipe；2nd, CNT/Co is prepared：Under ultrasonic assistant by acidifying after CNT evenly spread in distilled water, obtain carbon nanometer Pipe dispersion liquid, is then dissolved in cobalt nitrate in carbon nano tube dispersion liquid under ultrasonic state, obtains carbon nanotube mixture containing cobalt, To Deca sodium borohydride aqueous solution in carbon nanotube mixture containing cobalt under ultrasonic state, then filtered, using deionization Water is rinsed to solid phase filtrate, rinses 2～4 times, solid phase filtrate after being cleaned, then solid phase filtrate after cleaning is entered Row vacuum drying, obtains CNT/Co；The mass fraction of CNT after being acidified in carbon nano tube dispersion liquid described in step 2 For 0.1%～1%；The mass fraction of cobalt nitrate is 0.3%～3% in carbon nanotube mixture containing cobalt described in step 2； Sodium borohydride aqueous solution described in step 2 is (0.8～1.2) with the volume ratio of distilled water:10, and described sodium borohydride The mass fraction of sodium borohydride is 2%～30% in aqueous solution；3rd, MoS is loaded₂：It is under ultrasonic assistant that CNT/Co is uniform In being distributed to distilled water, CNT/Co dispersion liquids are obtained, then by MoS under ultrasonic state₂Powder body adds CNT/Co dispersion liquids, and Continual ultrasonic disperses 2h～5h, obtains mixture, and stratification takes subnatant and filtered, and solid formation is obtained, using deionization Water is rinsed to solid formation, rinses to liquid surface is filtered without metallic luster, solid formation after being cleaned, then to cleaning after Solid formation is vacuum dried, and obtains CNT/Co/MoS₂Composite, CNT/Co in the CNT/Co dispersion liquids described in step 3 Mass fraction be 0.1%～1%, MoS in the mixture described in step 3₂The mass fraction of powder body is 0.2%～3%.

2. a kind of CNT/Co/MoS according to claim 1₂The preparation method of composite, it is characterised in that in step one Described acid is concentrated nitric acid-concentrated sulphuric acid nitration mixture, the volume ratio 1 of described concentrated nitric acid and concentrated sulphuric acid:3, the quality of the concentrated nitric acid Fraction is 60%～68%, and the mass fraction of the concentrated sulphuric acid is 68%～75%.

3. a kind of CNT/Co/MoS according to claim 2₂The preparation method of composite, it is characterised in that in step one Described acid treatment concrete operations are as follows：CNT is put in concentrated nitric acid-concentrated sulphuric acid nitration mixture, the ultrasound in the case where temperature is for 50 DEG C 6h is processed, that is, completes acid treatment, the described quality of CNT and the volume ratio of concentrated nitric acid-concentrated sulphuric acid nitration mixture is 1g:40mL.

4. a kind of CNT/Co/MoS according to claim 1₂The preparation method of composite, it is characterised in that in step 2 Described vacuum drying concrete operations are as follows：6h is vacuum dried in the case where temperature is for 70 DEG C.

5. a kind of CNT/Co/MoS according to claim 1₂The preparation method of composite, it is characterised in that in step 2 The mass fraction of CNT is 0.1%～0.5% after being acidified in described carbon nano tube dispersion liquid.

6. a kind of CNT/Co/MoS according to claim 1₂The preparation method of composite, it is characterised in that in step 2 The mass fraction of cobalt nitrate is 0.6%～1.5% in described carbon nanotube mixture containing cobalt.

7. a kind of CNT/Co/MoS according to claim 1₂The preparation method of composite, it is characterised in that in step 2 Described sodium borohydride aqueous solution is 1 with the volume ratio of distilled water:Sodium borohydride in 10, and described sodium borohydride aqueous solution Mass fraction is 2%～10%.

8. a kind of CNT/Co/MoS according to claim 1₂The preparation method of composite, it is characterised in that in step 3 Described vacuum drying concrete operations are as follows：6h is vacuum dried in the case where temperature is for 70 DEG C.

9. a kind of CNT/Co/MoS according to claim 1₂The preparation method of composite, it is characterised in that in step 3 The mass fraction of CNT/Co is 0.1%～0.5% in described CNT/Co dispersion liquids.

10. a kind of CNT/Co/MoS according to claim 1₂The preparation method of composite, it is characterised in that in step 3 MoS in described mixture₂The mass fraction of powder body is 0.2%～1%.