CN104900867A - Preparation method of CNT/Co/MoS2 composite material - Google Patents
Preparation method of CNT/Co/MoS2 composite material Download PDFInfo
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- H01M4/00—Electrodes
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- H01M4/362—Composites
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- H—ELECTRICITY
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- H01M4/02—Electrodes composed of, or comprising, active material
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- H01M4/139—Processes of manufacture
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- H—ELECTRICITY
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- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
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- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/58—Selection of substances as active materials, active masses, active liquids of inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy; of polyanionic structures, e.g. phosphates, silicates or borates
- H01M4/581—Chalcogenides or intercalation compounds thereof
- H01M4/5815—Sulfides
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- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/58—Selection of substances as active materials, active masses, active liquids of inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy; of polyanionic structures, e.g. phosphates, silicates or borates
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Abstract
The invention relates to a preparation method of a CNT/Co/MoS2 composite material, relates to a modification method of molybdenum sulfide, and aims at solving the problems that according to the existing surface modification method of molybdenum sulfide, after modification, molybdenum sulfide still has hydrophobicity, or serious environment pollution problem is caused as a great deal of organic solvents are used in the existing surface modification method. The preparation method provided by the invention comprises the following steps: 1. performing acid treatment so as to obtain an acidized carbon nano tube; 2. preparing CNT/Co; and 3. loading MoS2 so as to obtain the CNT/Co/MoS2 composite material. The preparation method has the advantage that the surface of carbon nano tube can be uniformly coated by molybdenum sulfide. The technology is used for preparing the CNT/Co/MoS2 composite material.
Description
Technical field
The present invention relates to a kind of method of modifying of molybdenum sulfide.
Background technology
China's molybdenite produces aboundresources, molybdenite (MoS
2) there is much excellent character, such as lubrication, catalysis, stored energy and photoelectric property enjoy the favor of science and industrial circle.Particularly catalytic performance, compared with traditional catalyst, molybdenum sulfide not only has very high catalytic efficiency, and it effectively can also avoid the hydrogen sulfide poisoning phenomenon that the noble metals such as Pt often occur in catalytic process simultaneously.But, in the major applications process of molybdenum sulfide, as catalysis, stored energy, because molybdenite is water insoluble, the application of molybdenum sulfide directly can be limited.At present, main dependence is addressed this problem: 1) the synthesizing again of molybdate and sulphur source; 2) under organic solvent participates in, surfactant is to the surface modification of molybdenum sulfide.Rely on molybdate and sulphur source to the synthetic method again of molybdenum sulfide, although can obtain the higher molybdenum sulfide of catalytic activity, still there is hydrophobic problem in the molybdenum sulfide that the catalytic activity that the method obtains is higher; The second surface modifying treatment because relating to a large amount of organic solvent, then can cause serious problem of environmental pollution, is also difficult to batch production simultaneously.
Summary of the invention
There is modified molybdenum sulfide and still there is hydrophobic problem in the surface modifying treatment that the object of the invention is to solve existing molybdenum sulfide, or surface modifying treatment is because relating to a large amount of organic solvent, cause serious problem of environmental pollution, and a kind of CNT/Co/MoS is provided
2the preparation method of composite material.
A kind of CNT/Co/MoS
2the preparation method of composite material, specifically completes according to the following steps: one, acid treatment: carbon nano-tube is put into acid and carry out acid treatment, obtains carbon nano-tube after acidifying; Two, prepare CNT/Co: under ultrasonic assistant by acidifying after even carbon nanotube be distributed in distilled water, obtain carbon nano tube dispersion liquid, then under ultrasonic state, cobalt nitrate is dissolved in carbon nano tube dispersion liquid, obtain containing cobalt carbon nanotube mixture, sodium borohydride aqueous solution is dripped to containing in cobalt carbon nanotube mixture under ultrasonic state, then filter, deionized water is adopted to rinse solid phase filtrate, rinse 2 ~ 4 times, obtain cleaning rear solid phase filtrate, again vacuumize is carried out to solid phase filtrate after cleaning, obtain CNT/Co; In carbon nano tube dispersion liquid described in step 2, after acidifying, the quality of carbon nano-tube is divided is be 0.1% ~ 1%; Described in step 2 is 0.3% ~ 3% containing the mass fraction of cobalt nitrate in cobalt carbon nanotube mixture; The volume ratio of the sodium borohydride aqueous solution described in step 2 and distilled water is (0.8 ~ 1.2): 10, and in described sodium borohydride aqueous solution, the mass fraction of sodium borohydride is 2% ~ 30%; Three, load MoS
2: under ultrasonic assistant, CNT/Co is evenly spread in distilled water, obtain CNT/Co dispersion liquid, then under ultrasonic state, molybdenum sulfide powder is added CNT/Co dispersion liquid, and continual ultrasonic dispersion 2h ~ 5h, obtain mixture, stratification, get subnatant and filter, obtain solid formation, adopt deionized water to rinse solid formation, rinse to filtering liquid surperficial without metallic luster, obtain cleaning rear solid formation, again vacuumize is carried out to solid formation after cleaning, obtain CNT/Co/MoS
2composite material, in the CNT/Co dispersion liquid described in step 3, the mass fraction of CNT/Co is 0.1% ~ 1%, and in the mixture described in step 3, the mass fraction of molybdenum sulfide powder is 0.2% ~ 3%.
Advantage of the present invention: one, the present invention prepares CNT/Co/MoS
2directly use commercially available molybdenum sulfide powder to be raw materials in the method for composite material, course of reaction is normal temperature and pressure preparation process, and required consersion unit is also simple, and cost is low; Two, the present invention adopts magnetic synthetic method, and molybdenum sulfide is more even at the cladding ratio of carbon nano tube surface; Three, the present invention prepares CNT/Co/MoS
2the method of composite material is suitable for scale synthesis; Four, the CNT/Co/MoS for preparing of the present invention
2composite material has a wide range of applications in catalyst, solar cell, lithium ion battery, sensor.
Accompanying drawing explanation
Fig. 1 is the CNT/Co isothermal magnetic hysteresis loop figure that test one step 2 obtains;
Fig. 2 is the CNT/Co/MoS that test one obtains
2composite material isothermal magnetic hysteresis loop figure;
Fig. 3 is the cyclic voltammetric spectrogram of CNT/Co work electrode;
Fig. 4 is CNT/Co/MoS
2the cyclic voltammetric spectrogram of work electrode;
Fig. 5 is the CNT/Co Raman spectrogram that test one step 2 obtains;
Fig. 6 is the CNT/Co/MoS that test one obtains
2composite material Raman spectrogram;
Fig. 7 is CNT/Co/MoS
2work electrode is to H
2the I-t response curve of S alkaline solution;
Fig. 8 is the CNT/Co scanning electron microscope (SEM) photograph that test two step 2 obtains;
Fig. 9 is the CNT/Co/MoS of this test preparation
2composite material scanning electron microscope (SEM) photograph;
Figure 10 is that the CNT/Co that test two step 2 obtains projects Electronic Speculum figure;
Figure 11 is the CNT/Co/MoS of this test preparation
2composite material projection Electronic Speculum figure.
Embodiment
Embodiment one: present embodiment is a kind of CNT/Co/MoS
2the preparation method of composite material, specifically completes according to the following steps: one, acid treatment: carbon nano-tube is put into acid and carry out acid treatment, obtains carbon nano-tube after acidifying; Two, prepare CNT/Co: under ultrasonic assistant by acidifying after even carbon nanotube be distributed in distilled water, obtain carbon nano tube dispersion liquid, then under ultrasonic state, cobalt nitrate is dissolved in carbon nano tube dispersion liquid, obtain containing cobalt carbon nanotube mixture, sodium borohydride aqueous solution is dripped to containing in cobalt carbon nanotube mixture under ultrasonic state, then filter, deionized water is adopted to rinse solid phase filtrate, rinse 2 ~ 4 times, obtain cleaning rear solid phase filtrate, again vacuumize is carried out to solid phase filtrate after cleaning, obtain CNT/Co; In carbon nano tube dispersion liquid described in step 2, after acidifying, the quality of carbon nano-tube is divided is be 0.1% ~ 1%; Described in step 2 is 0.3% ~ 3% containing the mass fraction of cobalt nitrate in cobalt carbon nanotube mixture; The volume ratio of the sodium borohydride aqueous solution described in step 2 and distilled water is (0.8 ~ 1.2): 10, and in described sodium borohydride aqueous solution, the mass fraction of sodium borohydride is 2% ~ 30%; Three, load MoS
2: under ultrasonic assistant, CNT/Co is evenly spread in distilled water, obtain CNT/Co dispersion liquid, then under ultrasonic state, molybdenum sulfide powder is added CNT/Co dispersion liquid, and continual ultrasonic dispersion 2h ~ 5h, obtain mixture, stratification, get subnatant and filter, obtain solid formation, adopt deionized water to rinse solid formation, rinse to filtering liquid surperficial without metallic luster, obtain cleaning rear solid formation, again vacuumize is carried out to solid formation after cleaning, obtain CNT/Co/MoS
2composite material, in the CNT/Co dispersion liquid described in step 3, the mass fraction of CNT/Co is 0.1% ~ 1%, and in the mixture described in step 3, the mass fraction of molybdenum sulfide powder is 0.2% ~ 3%.
Embodiment two: the difference of present embodiment and embodiment one is: the acid described in step one is red fuming nitric acid (RFNA)-concentrated sulfuric acid nitration mixture, described red fuming nitric acid (RFNA) and concentrated sulfuric acid 1:3 by volume, the mass fraction of described red fuming nitric acid (RFNA) is 60% ~ 68%, and the mass fraction of the described concentrated sulfuric acid is 68% ~ 75%.Other are identical with embodiment one.
Embodiment three: one of present embodiment and embodiment one or two difference is: the acid treatment concrete operations described in step one are as follows: carbon nano-tube is put into red fuming nitric acid (RFNA)-concentrated sulfuric acid nitration mixture, ultrasonic process 6h at temperature is 50 DEG C, namely complete acid treatment, the volume ratio of the quality of described carbon nano-tube and red fuming nitric acid (RFNA)-concentrated sulfuric acid nitration mixture is 1g:40mL.Other are identical with embodiment one or two.
Embodiment four: one of present embodiment and embodiment one to three difference is: the vacuumize concrete operations described in step 2 are as follows: vacuumize 6h at temperature is 70 DEG C.Other are identical with embodiment one to three.
Embodiment five: one of present embodiment and embodiment one to four difference is: in the carbon nano tube dispersion liquid described in step 2, after acidifying, the quality of carbon nano-tube is divided is be 0.1% ~ 0.5%.Other are identical with embodiment one to four.
Embodiment six: one of present embodiment and embodiment one to five difference is: described in step 2 is 0.6% ~ 1.5% containing the mass fraction of cobalt nitrate in cobalt carbon nanotube mixture.Other are identical with embodiment one to five.
Embodiment seven: one of present embodiment and embodiment one to six difference is: the volume ratio of the sodium borohydride aqueous solution described in step 2 and distilled water is 1:10, and in described sodium borohydride aqueous solution, the mass fraction of sodium borohydride is 2% ~ 10%.Other are identical with embodiment one to six.
Embodiment eight: one of present embodiment and embodiment one to seven difference is: the vacuumize concrete operations described in step 3 are as follows: vacuumize 6h at temperature is 70 DEG C.Other are identical with embodiment one to seven.
Embodiment nine: one of present embodiment and embodiment one to eight difference is: in the CNT/Co dispersion liquid described in step 3, the mass fraction of CNT/Co is 0.1% ~ 0.5%.Other are identical with embodiment one to eight.
Embodiment ten: one of present embodiment and embodiment one to nine difference is: in the mixture described in step 3, the mass fraction of molybdenum sulfide powder is 0.2% ~ 1%.Other are identical with embodiment one to nine.
Adopt following verification experimental verification effect of the present invention
Test one: a kind of CNT/Co/MoS
2the preparation method of composite material, specifically completes according to the following steps: one, acid treatment: carbon nano-tube is put into acid and carry out acid treatment, obtains carbon nano-tube after acidifying, two, preparation CNT/Co: under ultrasonic assistant by acidifying after even carbon nanotube be distributed in distilled water, obtain carbon nano tube dispersion liquid, then under ultrasonic state, 600mg cobalt nitrate is dissolved in 100mL carbon nano tube dispersion liquid, obtain containing cobalt carbon nanotube mixture, drip to containing in cobalt carbon nanotube mixture the sodium borohydride solution that 10mL mass fraction is 5% under ultrasonic state, then filter, deionized water is adopted to rinse solid phase filtrate, rinse 3 times, obtain cleaning rear solid phase filtrate, again vacuumize is carried out to solid phase filtrate after cleaning, obtain CNT/Co, in carbon nano tube dispersion liquid described in step 2, after acidifying, the quality of carbon nano-tube is divided is be 0.1%, three, load MoS
2: under ultrasonic assistant, CNT/Co is evenly spread in distilled water, obtain CNT/Co dispersion liquid, then under ultrasonic state, molybdenum sulfide powder is added CNT/Co dispersion liquid, and continual ultrasonic dispersion 2h, obtain mixture, stratification, get subnatant and filter, obtain solid formation, adopt deionized water to rinse solid formation, rinse to filtering liquid surperficial without metallic luster, obtain cleaning rear solid formation, again vacuumize is carried out to solid formation after cleaning, obtain CNT/Co/MoS
2composite material, in the CNT/Co dispersion liquid described in step 3, the mass fraction of CNT/Co is 0.1%, and in the mixture described in step 3, the mass fraction of molybdenum sulfide powder is 0.2%.
Acid described in this test procedure one is red fuming nitric acid (RFNA)-concentrated sulfuric acid nitration mixture, described red fuming nitric acid (RFNA) and concentrated sulfuric acid 1:3 by volume, and the mass fraction of described red fuming nitric acid (RFNA) is 65%, and the mass fraction of the described concentrated sulfuric acid is 70%.
Acid treatment concrete operations described in this test procedure one are as follows: carbon nano-tube is put into red fuming nitric acid (RFNA)-concentrated sulfuric acid nitration mixture, ultrasonic process 6h at temperature is 50 DEG C, namely complete acid treatment, the volume ratio of the quality of described carbon nano-tube and red fuming nitric acid (RFNA)-concentrated sulfuric acid nitration mixture is 1g:40mL.
Vacuumize concrete operations described in this test procedure two are as follows: vacuumize 6h at temperature is 70 DEG C.
Vacuumize concrete operations described in this test procedure three are as follows: vacuumize 6h at temperature is 70 DEG C.
The CNT/Co/MoS that the CNT/Co obtain this test procedure two and this test obtain
2composite material carries out Magnetic Test, and as depicted in figs. 1 and 2, Fig. 1 is the CNT/Co isothermal magnetic hysteresis loop figure that test one step 2 obtains to test result; Fig. 2 is the CNT/Co/MoS that test one obtains
2composite material isothermal magnetic hysteresis loop figure; Can be found out by Fig. 1 and Fig. 2, the CNT/Co that this test procedure two obtains and the CNT/Co/MoS that this test obtains
2composite material is ferromagnetic substance, and has magnetic saturation phenomenon.When at the outer load MoS of CNT/Co
2time, the magnetic enhancement of material, magnetic moment increases, and the CNT/Co/MoS that this test obtains is described
2moS in composite material
2there is ferromagnetism.
The CNT/Co/MoS that the CNT/Co obtain this test procedure two and this test obtain
2composite material carries out electro-chemical test, and concrete grammar is as follows:
The CNT/Co that this test procedure of 2mg two obtains is dispersed in the Nafion-ethanolic solution of 10mL 0.5% (V/W), obtain dispersion liquid, again dispersant liquid drop is coated in clean glassy carbon electrode surface (glass-carbon electrode obtains clean glass-carbon electrode through polishing, cleaning successively), after natural drying, obtains CNT/Co work electrode.
By the CNT/Co/MoS that this test of 2mg obtains
2composite material is dispersed in the Nafion-ethanolic solution of 10mL 0.5% (V/W), obtain dispersion liquid, again dispersant liquid drop is coated in clean glassy carbon electrode surface (glass-carbon electrode obtains clean glass-carbon electrode through polishing, cleaning successively), after natural drying, obtains CNT/Co/MoS
2work electrode.
Respectively with CNT/Co work electrode and CNT/Co/MoS
2work electrode as work electrode, at the NaH of pH=7.0
2pO
4/ Na
2hPO
4carry out electro-chemical test in cushioning liquid, sweep speed: 50mV/s, as shown in Figure 3 and Figure 4, Fig. 3 is the cyclic voltammetric spectrogram of CNT/Co work electrode to test result; Fig. 4 is CNT/Co/MoS
2the cyclic voltammetric spectrogram of work electrode; Known by Fig. 3 and Fig. 4, CNT/Co/MoS
2the cyclic voltammetry spectrum characteristic peak shape of work electrode, position are not the result superposed on the cyclic voltammetric spectrogram basis of CNT/Co work electrode, but have the appearance at the skew (about 0.5V and 1.5V) at peak and new peak (about-1.8V), MoS is described
2not only successful load is in CNT/Co substrate, and MoS
2have mutually to act synergistically with CNT/Co substrate and produce.
The CNT/Co/MoS that the CNT/Co obtain this test procedure two and this test obtain
2composite material carries out Raman spectrum analysis, and as shown in Figure 5 and Figure 6, Fig. 5 is the CNT/Co Raman spectrogram that test one step 2 obtains to test result; Fig. 6 is the CNT/Co/MoS that test one obtains
2composite material Raman spectrogram; Known by the interpretation of result of Fig. 5 and Fig. 6 spectrogram: 1326cm
-1, 1575cm
-1near be feature D peak and the G peak of carbon nano-tube, 369cm
-1, 408cm
-1the peak of left and right is the E of molybdenum sulfide
2g 1and A
1gcharacteristic peak, with MoS
2normalized Raman spectrogram contrast find, E
2g 1there is blue shift and A in peak position
1gcharacteristic peak positions generation red shift, illustrates at CNT/Co/MoS
2moS in composite material
2layer structure change, become individual layer or few Rotating fields, i.e. sheet MoS from sandwich construction
2peel off.This kind of MoS
2stripping, cause sheet MoS
2the generation of edge defect or appearance are the CNT/Co/MoS that this test obtains
2moS in composite material
2produce ferromagnetic basic reason.
Test two: a kind of CNT/Co/MoS
2the preparation method of composite material, specifically completes according to the following steps: one, acid treatment: carbon nano-tube is put into acid and carry out acid treatment, obtains carbon nano-tube after acidifying, two, preparation CNT/Co: under ultrasonic assistant by acidifying after even carbon nanotube be distributed in distilled water, obtain carbon nano tube dispersion liquid, then under ultrasonic state, 1500mg cobalt nitrate is dissolved in 100mL carbon nano tube dispersion liquid, obtain containing cobalt carbon nanotube mixture, drip to containing in cobalt carbon nanotube mixture the sodium borohydride solution that 10mL mass fraction is 5% under ultrasonic state, then filter, deionized water is adopted to rinse solid phase filtrate, rinse 3 times, obtain cleaning rear solid phase filtrate, again vacuumize is carried out to solid phase filtrate after cleaning, obtain CNT/Co, in carbon nano tube dispersion liquid described in step 2, after acidifying, the quality of carbon nano-tube is divided is be 0.5%, three, load MoS
2: under ultrasonic assistant, CNT/Co is evenly spread in distilled water, obtain CNT/Co dispersion liquid, then under ultrasonic state, molybdenum sulfide powder is added CNT/Co dispersion liquid, and continual ultrasonic dispersion 2h, obtain mixture, stratification, get subnatant and filter, obtain solid formation, adopt deionized water to rinse solid formation, rinse to filtering liquid surperficial without metallic luster, obtain cleaning rear solid formation, again vacuumize is carried out to solid formation after cleaning, obtain CNT/Co/MoS
2composite material, in the CNT/Co dispersion liquid described in step 3, the mass fraction of CNT/Co is 0.2%, and in the mixture described in step 3, the mass fraction of molybdenum sulfide powder is 0.5%.
Acid described in this test procedure one is red fuming nitric acid (RFNA)-concentrated sulfuric acid nitration mixture, described red fuming nitric acid (RFNA) and concentrated sulfuric acid 1:3 by volume, and the mass fraction of described red fuming nitric acid (RFNA) is 65%, and the mass fraction of the described concentrated sulfuric acid is 70%.
Acid treatment concrete operations described in this test procedure one are as follows: carbon nano-tube is put into red fuming nitric acid (RFNA)-concentrated sulfuric acid nitration mixture, ultrasonic process 6h at temperature is 50 DEG C, namely complete acid treatment, the volume ratio of the quality of described carbon nano-tube and red fuming nitric acid (RFNA)-concentrated sulfuric acid nitration mixture is 1g:40mL.
Vacuumize concrete operations described in this test procedure two are as follows: vacuumize 6h at temperature is 70 DEG C.
Vacuumize concrete operations described in this test procedure three are as follows: vacuumize 6h at temperature is 70 DEG C.
Detect the CNT/Co/MoS of this test preparation
2composite material is to H
2the I-t response curve of S alkaline solution, detailed process is as follows:
By the CNT/Co/MoS that this test of 2mg obtains
2composite material is dispersed in the Nafion-ethanolic solution of 10mL 0.05% (V/W), obtains dispersion liquid, then 15 μ L dispersant liquid drops are coated in polishing glassy carbon electrode surface, and (glass-carbon electrode is successively through the α-Al of 0.3 μm
2o
3α-the Al of powder and 0.05 μm
2o
3powder polishing obtains the clean glass-carbon electrode of polishing), obtain CNT/Co/MoS after natural drying
2work electrode.
With CNT/Co/MoS
2work electrode as work electrode, by CNT/Co/MoS
2work electrode puts into H
2s alkaline solution (H
2s alkaline solution is by H
2s, NaOH and deionized water mix, and pH is 7.3) in, be to electrode with platinum electrode, calomel electrode is auxiliary electrode, carries out current-vs-time test.After test carries out 50 seconds, added 75 μ LH every 20 seconds
2s alkaline solution.As shown in Figure 7, Fig. 7 is CNT/Co/MoS to test result
2work electrode is to H
2the I-t response curve of S alkaline solution; As shown in Figure 7, CNT/Co/MoS
2work electrode at applied voltage about 0.5V, along with H
2being on the increase of S alkaline solution addition, current increment continues to increase, and stable electrical flow valuve also increases thereupon, and the response time is about 0.2 second, shows CNT/Co/MoS
2work electrode shows obvious H
2s sensitive property, proves CNT/Co/MoS prepared by this test
2composite material preparation can at H
2s or Na
2sensor part aspect is applied.
Fig. 8 is the CNT/Co scanning electron microscope (SEM) photograph that test two step 2 obtains; Fig. 9 is the CNT/Co/MoS of this test preparation
2composite material scanning electron microscope (SEM) photograph; Figure 10 is the CNT/Co transmission electron microscope picture that test two step 2 obtains; Figure 11 is the CNT/Co/MoS of this test preparation
2composite material transmission electron microscope picture; Known by Fig. 8-11, test CNT/Co that two step 2 obtain and CNT/Co/MoS prepared by this test
2the TEM figure nanotube walls thickness of composite material is even, and CNT surface Co and MoS is described
2be evenly distributed, CNT/Co/MoS
2pipe thickness be about about 12nm, the pipe thickness of CNT/Co is about about 7nm, and MoS is described
2evenly be coated in CNT substrate.
Claims (10)
1. a CNT/Co/MoS
2the preparation method of composite material, is characterized in that CNT/Co/MoS
2the preparation method of composite material completes according to the following steps: one, acid treatment: carbon nano-tube is put into acid and carry out acid treatment, obtains carbon nano-tube after acidifying; Two, prepare CNT/Co: under ultrasonic assistant by acidifying after even carbon nanotube be distributed in distilled water, obtain carbon nano tube dispersion liquid, then under ultrasonic state, cobalt nitrate is dissolved in carbon nano tube dispersion liquid, obtain containing cobalt carbon nanotube mixture, sodium borohydride aqueous solution is dripped to containing in cobalt carbon nanotube mixture under ultrasonic state, then filter, deionized water is adopted to rinse solid phase filtrate, rinse 2 ~ 4 times, obtain cleaning rear solid phase filtrate, again vacuumize is carried out to solid phase filtrate after cleaning, obtain CNT/Co; In carbon nano tube dispersion liquid described in step 2, after acidifying, the quality of carbon nano-tube is divided is be 0.1% ~ 1%; Described in step 2 is 0.3% ~ 3% containing the mass fraction of cobalt nitrate in cobalt carbon nanotube mixture; The volume ratio of the sodium borohydride aqueous solution described in step 2 and distilled water is (0.8 ~ 1.2): 10, and in described sodium borohydride aqueous solution, the mass fraction of sodium borohydride is 2% ~ 30%; Three, load MoS
2: under ultrasonic assistant, CNT/Co is evenly spread in distilled water, obtain CNT/Co dispersion liquid, then under ultrasonic state, molybdenum sulfide powder is added CNT/Co dispersion liquid, and continual ultrasonic dispersion 2h ~ 5h, obtain mixture, stratification, get subnatant and filter, obtain solid formation, adopt deionized water to rinse solid formation, rinse to filtering liquid surperficial without metallic luster, obtain cleaning rear solid formation, again vacuumize is carried out to solid formation after cleaning, obtain CNT/Co/MoS
2composite material, in the CNT/Co dispersion liquid described in step 3, the mass fraction of CNT/Co is 0.1% ~ 1%, and in the mixture described in step 3, the mass fraction of molybdenum sulfide powder is 0.2% ~ 3%.
2. a kind of CNT/Co/MoS according to claim 1
2the preparation method of composite material, it is characterized in that the acid described in step one is red fuming nitric acid (RFNA)-concentrated sulfuric acid nitration mixture, described red fuming nitric acid (RFNA) and concentrated sulfuric acid 1:3 by volume, the mass fraction of described red fuming nitric acid (RFNA) is 60% ~ 68%, and the mass fraction of the described concentrated sulfuric acid is 68% ~ 75%.
3. a kind of CNT/Co/MoS according to claim 2
2the preparation method of composite material, it is characterized in that the acid treatment concrete operations described in step one are as follows: carbon nano-tube is put into red fuming nitric acid (RFNA)-concentrated sulfuric acid nitration mixture, ultrasonic process 6h at temperature is 50 DEG C, namely complete acid treatment, the volume ratio of the quality of described carbon nano-tube and red fuming nitric acid (RFNA)-concentrated sulfuric acid nitration mixture is 1g:40mL.
4. a kind of CNT/Co/MoS according to claim 1
2the preparation method of composite material, is characterized in that the vacuumize concrete operations described in step 2 are as follows: vacuumize 6h at temperature is 70 DEG C.
5. a kind of CNT/Co/MoS according to claim 1
2the preparation method of composite material, it is characterized in that the quality of carbon nano-tube after acidifying in the carbon nano tube dispersion liquid described in step 2 is divided is be 0.1% ~ 0.5%.
6. a kind of CNT/Co/MoS according to claim 1
2the preparation method of composite material, is characterized in that the mass fraction containing cobalt nitrate in cobalt carbon nanotube mixture described in step 2 is 0.6% ~ 1.5%.
7. a kind of CNT/Co/MoS according to claim 1
2the preparation method of composite material, it is characterized in that the volume ratio of the sodium borohydride aqueous solution described in step 2 and distilled water is 1:10, and in described sodium borohydride aqueous solution, the mass fraction of sodium borohydride is 2% ~ 10%.
8. a kind of CNT/Co/MoS according to claim 1
2the preparation method of composite material, is characterized in that the vacuumize concrete operations described in step 3 are as follows: vacuumize 6h at temperature is 70 DEG C.
9. a kind of CNT/Co/MoS according to claim 1
2the preparation method of composite material, is characterized in that the mass fraction of CNT/Co in the CNT/Co dispersion liquid described in step 3 is 0.1% ~ 0.5%.
10. a kind of CNT/Co/MoS according to claim 1
2the preparation method of composite material, is characterized in that the mass fraction of molybdenum sulfide powder in the mixture described in step 3 is 0.2% ~ 1%.
Priority Applications (1)
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| CN106611837A (en) * | 2015-10-27 | 2017-05-03 | 上海交通大学 | Cobalt-intercalated molybdenum sulfide secondary battery material and preparation method and application thereof |
| CN106925303A (en) * | 2017-04-24 | 2017-07-07 | 吉林师范大学 | A kind of MoS2/CNTs/C60Composite photo-catalyst and preparation method thereof |
| CN107834040A (en) * | 2017-09-28 | 2018-03-23 | 浙江工业大学 | A kind of lithium battery porous carbon negative pole material of bio-based N doping of load molybdenum disulfide and preparation method thereof |
| CN108220828A (en) * | 2018-01-30 | 2018-06-29 | 东莞颠覆产品设计有限公司 | A kind of amorphous alloy composite material and its preparation method and application |
| CN109273726A (en) * | 2018-02-08 | 2019-01-25 | 成都理工大学 | A kind of carbon coated air electrode material and its preparation method and application |
| CN109786673A (en) * | 2019-01-10 | 2019-05-21 | 湘潭大学 | A kind of preparation process of lithium ion battery flexible compound self-supporting electrode |
| CN110380028A (en) * | 2019-07-08 | 2019-10-25 | 武汉理工大学 | A kind of CNT/MoS2Lithium ion battery negative material and preparation method thereof |
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| CN115155621A (en) * | 2022-05-19 | 2022-10-11 | 福州大学 | Co-MoS 2 /CNT (carbon nano tube) photocatalytic modified film as well as preparation method and application thereof |
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| CN109786673A (en) * | 2019-01-10 | 2019-05-21 | 湘潭大学 | A kind of preparation process of lithium ion battery flexible compound self-supporting electrode |
| CN110380028A (en) * | 2019-07-08 | 2019-10-25 | 武汉理工大学 | A kind of CNT/MoS2Lithium ion battery negative material and preparation method thereof |
| CN110380028B (en) * | 2019-07-08 | 2022-09-09 | 武汉理工大学 | CNT/MoS 2 Lithium ion battery cathode material and preparation method thereof |
| CN111250112A (en) * | 2020-03-19 | 2020-06-09 | 武汉理工大学 | High-performance electro-catalytic hydrogen evolution heterogeneous composite catalyst and preparation method thereof |
| CN115155621A (en) * | 2022-05-19 | 2022-10-11 | 福州大学 | Co-MoS 2 /CNT (carbon nano tube) photocatalytic modified film as well as preparation method and application thereof |
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