CN105460921B - A kind of selenizing molybdenum nanometer sheet/graphene nano belt composite and preparation method thereof - Google Patents
A kind of selenizing molybdenum nanometer sheet/graphene nano belt composite and preparation method thereof Download PDFInfo
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- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
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Abstract
The invention belongs to Transition-metal dichalcogenide carbon material technical field, specially a kind of selenizing molybdenum/graphene nano belt composite and preparation method thereof.The present invention prepares graphene nanobelt by solution oxide method, then by solvent-thermal method on graphene nano band growth in situ selenizing molybdenum nanometer sheet.Graphene nanobelt prepared by the present invention has the advantages that chemical property is stable, draw ratio is high；Composite prepared by the present invention has the characteristics of morphology controllable, and selenizing molybdenum nanometer sheet is equably supported on graphene nano band, restrained effectively the selenizing molybdenum reunion of itself, takes full advantage of the unique high-specific surface area of graphene nanobelt and high conductivity.Selenizing molybdenum nanometer sheet/graphene nano belt composite prepared by the present invention can turn into a kind of preferably high-performance electric chemistry liberation of hydrogen catalysis material, and the electrode material of the new energy devices such as lithium ion battery and solar cell.
Description
Technical field
The invention belongs to Transition-metal dichalcogenide-carbon material technical field, and in particular to and a kind of selenizing molybdenum nanometer sheet/
Graphene nano belt composite and preparation method thereof.
Technical background
Graphene nanobelt is a kind of accurate one-dimensional c-based nanomaterial, and it has many excellent physical and chemical performances, such as
Higher electric conductivity, excellent mechanical property, special edge effect and good chemical stability etc..These special natures make
Before it all has extremely wide application in the field such as energy conversion and storage, electronic sensor, high molecule nano composite material
Scape, turn into one of study hotspot in carbon nanomaterial field.
Selenizing molybdenum is a kind of typical Transition-metal dichalcogenide, and it belongs to hexagonal crystal system, is very strong Se- in layer
Mo-Se covalent bonds, interlayer are weaker Van der Waals forces, and thickness in monolayer is about 0.65 nm.Research shows, the work of selenizing molybdenum exposure
Property edge has catalytic activity for hydrogen evolution, and the Gibbs free energy of its liberation of hydrogen is lower than molybdenum disulfide, therefore theoretical liberation of hydrogen mistake
Current potential is lower, and catalytic effect is more preferable.But pure selenium molybdenum is easy to reunite, and the inert endothecium structure of its preferred growth, rather than
Active lamella edge, substantial amounts of aggregate also further suppress the exposure at active edge, along with its poor electric conductivity, selenium
The excellent properties for changing molybdenum will be unable to be fully used.Therefore, by selenizing molybdenum and the compound tool of base material of other high conductivity
It is significant.
A kind of new selenizing molybdenum/graphene nanobelt composite wood is prepared by simple technological design in the present invention
Material.The composite has following advantage：The unique edge effect of graphene nanobelt can provide more for the growth of selenizing molybdenum
More avtive spots, the active edge of selenizing molybdenum nanometer sheet is set more fully to be exposed；Graphene nanobelt is excellent to lead
Electrical property is advantageous to the transmission of electronics, can improve the overall electric conductivity of composite；The thin slice Rotating fields of graphene nanobelt have
Beneficial to the migration of electrolyte ion in electrochemical process, so as to reduce its contact internal resistance with solution.And selenizing molybdenum nanometer sheet sheet
Body possesses excellent catalytic activity and energy stores performance, therefore both are carried out into effectively compound achievable good synergy,
To prepare the composite of excellent performance.
The content of the invention
It is an object of the invention to provide a kind of cost is cheap, selenizing molybdenum nanometer sheet/graphene of electrochemical performance
Nanometer belt composite and preparation method thereof.
Selenizing molybdenum/graphene nano belt composite provided by the present invention, it is molten by a step by selenium powder and sodium molybdate
The hot method of agent growth in situ selenizing molybdenum nanometer sheet on the graphene nano band with special band edge is prepared；It prepares former
Material composition includes：CNT（Single wall or more walls）, potassium permanganate, the concentrated sulfuric acid, phosphoric acid, selenium powder, sodium molybdate, and hydrazine hydrate.
The preparation method of selenizing molybdenum/graphene nano belt composite provided by the present invention, including：Pass through solution oxide
Method prepares graphene nanobelt；By solvent-thermal method on graphene nano band growth in situ selenizing molybdenum nanometer sheet；Specific steps
It is as follows：
（1）CNT is scattered in the 95%-98% concentrated sulfuric acid, 85% phosphoric acid is added after being uniformly dispersed, constantly
Stirring obtains homogeneous dispersion liquid；
（2）Potassium permanganate is added in above-mentioned dispersion liquid, is stirred continuously；
（3）Reaction system is to slowly warm up to 60-80 DEG C, after temperature stabilization, is incubated 2-3h；And it is stirred continuously；
（4）The mixed solution of gained is naturally cooled into room temperature, is subsequently poured into the frozen water containing hydrogen peroxide, it is overnight to put
Put, make its natural subsidence；
（5）Obtained sediment is washed repeatedly with aqueous hydrochloric acid solution, then washed with the mixed solution of ethanol/ether more
It is secondary；
（6）Centrifugal drying obtains solid oxidation graphene nanobelt；
（7）Stannic oxide/graphene nano band is scattered in organic solvent, ultrasonic disperse, it is steady to obtain stannic oxide/graphene nano band
Determine dispersion liquid；
（8）Selenium powder is dissolved in hydrazine hydrate, heating stirring, is allowed to be uniformly dispersed；
（9）Sodium molybdate is dissolved in minor amount of water, ultrasonic disperse, is allowed to be uniformly dispersed；
（10）By step（8）、（9）The dispersion liquid of preparation is added in stannic oxide/graphene nano band organic dispersions, ultrasound point
Dissipate uniform；
（11）By step（10）The resulting mixing containing stannic oxide/graphene nano band, sodium molybdate, selenium powder and hydrazine hydrate
Liquid is poured into water heating kettle, and solvent thermal reaction for a period of time, that is, obtains selenizing molybdenum/graphene nanobelt composite wood at a certain temperature
Material；
（12）By the black precipitate deionized water and ethanol of the selenizing being prepared molybdenum/graphene nano belt composite
Washing is multiple repeatedly, then dries, standby.
In the present invention, described stannic oxide/graphene nano band is radially to cut off CNT by solution oxide method to be prepared into
Arrive, the method refers to the Al of patent US 2010/0105834.
In the present invention, described selenizing molybdenum nanometer sheet is formed by solvent-thermal method growth, meanwhile, hydrazine hydrate makes graphite oxide
Alkene nanobelt is reduced into graphene nanobelt.The solvent that solvent-thermal method uses isN,N-Dimethylformamide,N,N-Dimethyl second
Acid amides orN-Methyl pyrrolidone.
In the present invention, step（1）The concentration of described CNT is 3-5 mg/mL, the concentrated sulfuric acid and phosphoric acid volume ratio
For 8:1-10:1, preferably 9:1.
In the present invention, step（2）The quality of described potassium permanganate is 2-5 times of CNT dosage.
In the present invention, step（3）Described temperature is 60-80 DEG C, and the time of insulation is 2-3h.
In the present invention, step（5）Described aqueous hydrochloric acid solution weight concentration is 5-20%.
In the present invention, step（7）Concentration of the described stannic oxide/graphene nano with dispersion liquid is 0.5-2 mg/mL, preferably
1-1.5 mg/mL。
In the present invention, step（8）Described selenium powder is dispersed in hydrazine hydrate, concentration is in the case where heating-up temperature is 60-80 DEG C
1-6 mg/mL。
In the present invention, step（9）Described sodium molybdate and the mol ratio of selenium powder are 1:1.8-1:2.4, preferably 1:2, solvent
The dosage of water should be lacked as far as possible, and sodium molybdate is completely dissolved.
In the present invention, step（11）Described reaction temperature is 180 ~ 220 DEG C, and the reaction time is 10 ~ 24 h.
Use transmission electron microscope（TEM）, SEM（SEM）, X-ray diffractometer（XRD）, electrochemistry work
Make station to characterize the structure and morphology of selenizing molybdenum/graphene nano belt composite that the present invention is obtained, its result is as follows：
（1）TEM test results show, multi-walled carbon nanotube, inner layer wall and sky have successfully been peeled off with the method radially cut off
The border of chamber substantially disappears；
（2）SEM test results show：In the composite, selenizing molybdenum nanometer sheet is equably supported on graphene nanobelt
Surface, the unique edge of prepared graphene nanobelt provides more active sites for the growth of molybdenum disulfide nano sheet
Point, the edge for the molybdenum disulfide nano sheet layer for making to have catalytic activity are sufficiently exposed.The banding side of graphene nanobelt
Edge structure assigns its more flexible adjustability, and this is also that it is different from the most substantive characteristics of Sheet Graphite alkene.Prepared selenium
Change molybdenum to be equably grown on graphene nano band, preferably inhibit the reunion of molybdenum disulfide itself；
（3）XRD test results show that graphene nanobelt has a wider diffraction maximum in 2 θ=26.0 °, corresponds to
Its（002）Crystal face.In 2 θ=13.7 °, 26.4 °, 32.2 °, 37.3 °, 53.8 °, 56.4 °, 60.9 ° and 67.0 ° are spread out selenizing molybdenum
Hexagonal structure 2H-MoSe can be corresponded respectively to by penetrating peak2's（002）,（004）,（100）,（103）,（106）,（008）,（107）
With（202）Crystal face.Prepared selenizing molybdenum nanometer sheet/graphene nano belt composite shows the characteristic peak of selenizing molybdenum,
Illustrate that selenizing molybdenum nanometer sheet is successfully carried on graphene nano band；
（4）Electrochemical workstation test result shows, prepared selenizing molybdenum nanometer sheet/graphene nano belt composite
With excellent electrocatalytic hydrogen evolution performance, its catalytic hydrogen evolution overpotential is -0.1 V, and compared with pure selenizing molybdenum, either
Originate the liberation of hydrogen current density under overpotential, or same potential, selenizing molybdenum nanometer sheet/graphene nano belt composite all bodies
Reveal more excellent performance.
The advantage of the invention is that：
1st, preparation process is simple, easily operated, is a kind of effective efficiently preparation method；
2nd, experimental design is ingenious：
First, the substrate of selection is graphene nanobelt.Its unique draw ratio and marginal texture impart its high ratio
Surface area, and provide more sites and grown for selenizing molybdenum nanometer sheet.Graphene nanobelt has excellent electric conductivity, its
Lamellar structure make it that electronics and ion can with effective and rapid transmit during electro-catalysis, can further improve urging for selenizing molybdenum
Change hydrogen evolution activity；
Second, the compound of quasi one-dimensional material and two-dimensional material is realized by simple solvent thermal process so that both
Advantage is given full play to, so as to construct the composite with excellent properties.
Selenizing molybdenum nanometer sheet/graphene nano belt composite prepared by the present invention, can be used as high-performance liberation of hydrogen catalyst
The ideal electrode material of the novel energy such as material and lithium ion battery, solar cell.
Brief description of the drawings
Fig. 1 is that material TEM schemes in the present invention.Wherein,（A）Multi-walled carbon nanotube,（B）Graphene nanobelt.
Fig. 2 is GNR@MoSe of the present invention2The SEM figures of -1 composite.
Fig. 3 is the XRD of selenizing molybdenum nanometer sheet/graphene nano belt composite.
Fig. 4 is GNR@MoSe of the present invention2The linear sweep voltammetry for electrochemistry liberation of hydrogen catalyst of -1 composite is bent
Line（LSV）.
Embodiment
With reference to instantiation, the present invention is expanded on further.It should be understood that these embodiments be merely to illustrate the present invention and
It is not used in limitation the scope of the present invention.In addition, after the content of the invention lectured has been read, those skilled in the art can be right
The present invention makes various changes or modification, and these equivalent form of values equally fall within the application appended claims limited range.
Embodiment 1, the present embodiment comprise the following steps：
（1）150 mg multi-walled carbon nanotubes are scattered in 98% concentrated sulfuric acid, 85% phosphorus is added after being uniformly dispersed
Acid, it is stirred continuously to obtain homogeneous dispersion liquid in the process；
（2）750 mg potassium permanganate are added in above-mentioned dispersion liquid, is added portionwise, is stirred continuously；
（3）Reaction system is to slowly warm up to 70 DEG C, after temperature stabilization, insulation a period of time, and be stirred continuously；
（4）The mixed dispersion liquid of gained is naturally cooled into room temperature, is subsequently poured into the frozen water of the hydrogen peroxide containing 7mL50%,
Placement overnight, make its natural subsidence；
（5）Obtained sediment is washed repeatedly with 10% aqueous hydrochloric acid solution, then washed with the mixed solution of ethanol/ether
Wash repeatedly；
（6）Centrifugal drying obtains solid oxidation graphene nanobelt, is designated as GONR；
（7）Stannic oxide/graphene nano band is scattered inN,N-In dimethylformamide, ultrasound obtains 1 mg/ of stable dispersion
ML stannic oxide/graphene nano band；
（8）Selenium powder is dissolved in hydrazine hydrate, is made into 4 mg/mL dispersion liquids, heating stirring for a period of time, is allowed to scattered equal
It is even, take 1.25 mL stand-by；
（9）7.66 mg sodium molybdates are dissolved in 200 μ L water, ultrasound is allowed to be uniformly dispersed；
（10）Will（8）、（9）The dispersion liquid of preparation is added in 10 mL stannic oxide/graphene nanos band organic dispersions, ultrasound point
Dissipate uniform；
（11）The made mixed liquor containing stannic oxide/graphene nano band, sodium molybdate, selenium powder and hydrazine hydrate got ready is poured into
In water heating kettle, the h of solvent thermal reaction 12 at 200 DEG C, that is, selenizing molybdenum/graphene nano belt composite GNR MoSe are obtained2-
0.5；
（12）By the black precipitate deionized water and ethanol of the selenizing being prepared molybdenum/graphene nano belt composite
Washing is multiple repeatedly, then dries, standby.
Embodiment 2, the dosage of the selenium powder dispersion liquid in embodiment 1 is changed into 2.5 mL, the quality of sodium molybdate is changed into 15.32
Mg, with embodiment 1, the composite finally obtained is designated as GNR@MoSe for remaining2-1。
Embodiment 3, the dosage of the selenium powder dispersion liquid in embodiment 1 is changed into 5 mL, the quality of sodium molybdate is changed into 30.64
Mg, with embodiment 1, the composite finally obtained is designated as GNR@MoSe for remaining2-2。
Embodiment 4, the dosage of the potassium permanganate in embodiment 1 being changed into 450 mg, solvent heat temperature is changed into 220 DEG C, its
For Yu Jun with embodiment 1, the composite finally obtained is designated as GNR MoSe2-3。
Claims (10)
- A kind of 1. preparation method of selenizing molybdenum/graphene nano belt composite, it is characterised in that：Prepared by solution oxide method Obtain graphene nanobelt；Again by a step solvent-thermal method on graphene nano band growth in situ selenizing molybdenum nanometer sheet；Specifically Step is as follows：（1）CNT is scattered in the 95%-98% concentrated sulfuric acid, 85% phosphoric acid is added after being uniformly dispersed, is constantly stirred Mix, obtain homogeneous dispersion liquid；（2）Potassium permanganate is added in above-mentioned dispersion liquid, is stirred continuously；（3）Reaction system is to slowly warm up to 60-80 DEG C, after temperature stabilization, is incubated 2-3h；And it is stirred continuously；（4）The mixed solution of gained is naturally cooled into room temperature, is subsequently poured into the frozen water containing hydrogen peroxide, placement overnight, is made Its natural subsidence；（5）Obtained sediment is washed repeatedly with aqueous hydrochloric acid solution, then washed repeatedly with the mixed solution of ethanol/ether；（6）Centrifugal drying obtains solid oxidation graphene nanobelt；（7）Stannic oxide/graphene nano band is scattered in organic solvent, ultrasonic disperse, obtains stable point of stannic oxide/graphene nano band Dispersion liquid；（8）Selenium powder is dissolved in hydrazine hydrate, heating stirring, is allowed to be uniformly dispersed；（9）Sodium molybdate is dissolved in minor amount of water, ultrasonic disperse, is allowed to be uniformly dispersed；（10）By step（8）、（9）The dispersion liquid of preparation is added in stannic oxide/graphene nano band organic dispersions, and ultrasonic disperse is equal It is even；（11）By step（10）The resulting mixed liquor containing stannic oxide/graphene nano band, sodium molybdate, selenium powder and hydrazine hydrate falls Enter in water heating kettle, solvent thermal reaction for a period of time, that is, obtains selenizing molybdenum/graphene nano belt composite at a certain temperature；（12）By the black precipitate deionized water of the selenizing being prepared molybdenum/graphene nano belt composite and ethanol repeatedly Washing is multiple, then dries, standby.
- 2. the preparation method of selenizing molybdenum/graphene nano belt composite according to claim 1, it is characterised in that molten The solvent that the hot method of agent uses isN,N-Dimethylformamide,N,N-Dimethyl acetamide orN-Methyl pyrrolidone.
- 3. the preparation method of selenizing molybdenum/graphene nano belt composite according to claim 1, it is characterised in that step Suddenly（1）Described in the concentration of CNT be 3-5 mg/mL, the volume ratio of the concentrated sulfuric acid and phosphoric acid is 8:1-10:1.
- 4. the preparation method of selenizing molybdenum/graphene nano belt composite according to claim 1, it is characterised in that step Suddenly（2）Described in the quality of potassium permanganate be 2-5 times of CNT dosage.
- 5. the preparation method of selenizing molybdenum/graphene nano belt composite according to claim 1, it is characterised in that step Suddenly（5）Described in aqueous hydrochloric acid solution weight concentration be 5-20%；Step（7）Described in stannic oxide/graphene nano band dispersion liquid Concentration be 0.5-2 mg/mL.
- 6. the preparation method of selenizing molybdenum/graphene nano belt composite according to claim 1, it is characterised in that step Suddenly（8）Described in selenium powder heating-up temperature be 60-80 DEG C at, be dispersed in hydrazine hydrate, concentration is 1-6 mg/mL.
- 7. the preparation method of selenizing molybdenum/graphene nano belt composite according to claim 1, it is characterised in that step Suddenly（9）Described in sodium molybdate and the mol ratio of selenium powder be 1:1.8-1:2.4, the dosage of aqueous solvent only need to be completely molten by sodium molybdate Solution.
- 8. the preparation method of selenizing molybdenum/graphene nano belt composite according to claim 1, it is characterised in that step Suddenly（11）Described in solvent thermal reaction, its reaction temperature be 180 ~ 220 DEG C, the reaction time is 10 ~ 24 h.
- A kind of 9. selenizing molybdenum/graphene nano belt composite being prepared by one of the claim 1-8 preparation methods.
- 10. selenizing molybdenum/graphene nano belt composite as claimed in claim 9 as high-performance liberation of hydrogen catalyst material with And the application of the electrode material of lithium ion battery, solar cell.
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| CN108641261A (en) * | 2018-05-17 | 2018-10-12 | 西北工业大学 | Amido modified graphene/class graphene MoSe2/ Bismaleimide composites and preparation method |
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