CN105206807A - MoS2/C superlattice heterojunction nano-sheet self-assembled nano-tube as well as preparation method and application thereof - Google Patents
MoS2/C superlattice heterojunction nano-sheet self-assembled nano-tube as well as preparation method and application thereof Download PDFInfo
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- CN105206807A CN105206807A CN201510563691.0A CN201510563691A CN105206807A CN 105206807 A CN105206807 A CN 105206807A CN 201510563691 A CN201510563691 A CN 201510563691A CN 105206807 A CN105206807 A CN 105206807A
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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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Abstract
The invention discloses a MoS2/C superlattice heterojunction nano-sheet self-assembled nano-tube as well as a preparation method and an application thereof. The MoS2/C superlattice heterojunction nano-sheet self-assembled nano-tube is characterized by being formed by self-assembling nano-sheets, wherein each nano-sheet is formed by laminating two-dimensional MoS2 molecule layers, a C atomic layer is embedded between two adjacent MoS2 molecular layers to form a MoS2/C superlattice heterojunction. The MoS2/C superlattice heterojunction can be used as a cathode material of a sodium ion battery with high cycling stability and rate capacity. By virtue of the thermal reaction of solvent, octylamine molecules is embedded between the MoS2 layers, the interlayer distance is increased, then the octylamine molecules are carbonated between the MoS2 layers to be converted into C to form a MoS2/C superlattice structure. Compared with the ordinary MoS2 material, the MoS2/C superlattice heterojunction nano-sheet self-assembled nano-tube has advantages of good conductivity, stable structure, unlikeliness in concentration and the like.
Description
Technical field
The present invention relates to a kind of MoS
2/ C superlattice heterojunction nanometer sheet self-assembled nanometer pipe and its preparation method and application, belongs to technical field of nano material.
Background technology
In recent years, along with the rise of Graphene research boom, the two-dimensional layer transition metal two chalcogen compound MX of class Graphene
2(M=Mo, W; X=S, Se), as MoS
2, WS
2, MoSe
2deng, cause the great interest of academia, become the focus of current research.The thickness of two-dimensional layered structure crystal is reduced to individual layer or which floor, can marked change be there is in electricity and optical property, individual layer transition metal two chalcogen compound has sandwich structure, and therebetween central layer is made up of metallic atom, and two-layer is up and down be made up of sulfur family atom (S, Se).Be rely on covalent bond to connect within individual layer, and the interlayer of sandwich construction rely on Van der Waals force to connect, layer structure MX
2there is the features such as ultrathin, two-dimensional appearance, specific area be large.MoS
2in fields such as lubricant, energy storage, electrochemical catalysis and opto-electronic devices, there is important application prospect.But stratiform MoS
2material band gap is comparatively large, poor electric conductivity.Due to the anisotropy of crystal, electronics is at MoS
2between molecular layer, the transmission in (c-axis direction) is particularly difficult, has a strong impact on and limit it produces the electronic devices such as hydrogen performance in sodium (lithium) ion battery, electrochemistry.In addition, block MoS
2the interlamellar spacing of material is 0.615nm, cannot meet sodium (lithium) the ion fast transport of high-performance sodium (lithium) ion battery charge and discharge process demand.Therefore, explore a kind of method that is simple, that be applicable to large-scale production and prepare the good and MoS of interlamellar spacing broadening of electric conductivity
2nanostructure has important practical significance and using value.
Summary of the invention
The present invention is the weak point for avoiding existing for above-mentioned prior art, provides a kind of MoS
2/ C superlattice heterojunction nanometer sheet self-assembled nanometer pipe and preparation method thereof, is intended to solve block MoS
2the problems such as poorly conductive, interlamellar spacing are narrow, easy reunion, improve MoS simultaneously
2the charge-discharge performance of electrode material in sodium-ion battery.
Technical solution problem of the present invention adopts following technical scheme:
MoS of the present invention
2/ C superlattice heterojunction nanometer sheet self-assembled nanometer pipe, its feature is: described nanotube is made up of nanometer sheet self assembly, and which floor MoS is described nanometer sheet be by
2molecular layer superposition is formed, adjacent MoS
2between molecular layer, intercalation has monolayer carbon atomic layer, forms MoS
2/ C superlattice heterojunction.Form MoS
2the adjacent MoS of nanometer sheet
2spacing between molecular layer is 0.98nm.Adjacent MoS in described superlattice heterojunction
2the interlamellar spacing of molecular layer and carbon atomic layer is 0.49nm.
Above-mentioned MoS
2the preparation method of/C superlattice heterojunction nanometer sheet self-assembled nanometer pipe, its feature is to carry out as follows:
A, take S powder 1-2mmol, and join in 10-15mL octylame solution, continue to add 0.4-0.6mmol molybdenum source, stir 0-10 minute under normal temperature, then add 10-20mL anhydrous ethanol solvent, obtain mixed solution; Described mixed solution is transferred in reactor and at 170-200 DEG C, reacts 3-8 hour, obtain initial product;
B, by described initial product under the protection of argon hydrogen, 300-700 DEG C of annealing in process 1 hour, obtains target product.
Described molybdenum source is ammonium molybdate or molybdenum trioxide.
The invention also discloses above-mentioned MoS
2the application of/C superlattice heterojunction nanometer sheet self-assembled nanometer pipe, its feature is: for the negative material as sodium-ion battery.
The present invention is to this MoS
2the formation mechenism of/C superlattice heterojunction nanometer sheet self-assembled nanometer pipe have also been made research: in the middle of experiment, and sulphur powder is easy to be dissolved in the middle of octylame and forms red tan solution, indicates the formation of S-octylame complex.Again by MoO
3powder is dissolved in the mixed solution of octylame and absolute ethyl alcohol gradually, forms red solution at 170-200 DEG C of solvent thermal reaction after 60 minutes, now there is no precipitation and is formed, show MoO
3powder dissolves completely and defines Mo-octylame complex; When reaching 80 minutes when reacted, Mo-octylame complex and S-octylame complex react further and form the coated MoS of octylame
2nanometer sheet, these nanometer sheet are easily reunited (as Suo Shi Fig. 1 (a)); When reaching 100 minutes when reacted, the MoS that octylame is coated
2nanometer sheet self assembly, has the pointed aggregation of one dimension to form (as Suo Shi Fig. 1 (b)); Last till 120 minutes when reacted, have nanotube to occur, but now tube diameters less (about 40nm) (as Suo Shi Fig. 1 (c)); Along with the reaction time extend to 180 minutes time, the diameter of nanotube is increased to 130nm, obtain initial product (as Suo Shi Fig. 1 (d)).After centrifugal drying, gained initial product is the nanotube of nanometer sheet self assembly.Wherein nanotube is by MoS
2nanometer sheet self assembly is formed, MoS
2nanometer sheet is by multilayer MoS
2molecular layer superposition is formed, adjacent MoS
2octylame molecule is embedded with between molecular layer.To initial product MoS
2nanotube 300-700 DEG C annealing in process, makes the carbonization of octylame molecule, obtains MoS
2/ C superlattice heterojunction nanometer sheet self-assembled nanometer pipe (as shown in Figure 2).
Compared with the prior art, beneficial effect of the present invention is embodied in:
1, the invention provides a kind of MoS
2the preparation method of/C superlattice heterojunction nanometer sheet self-assembled nanometer pipe, makes two-dimensional structure MoS by solvent thermal reaction
2interlamellar spacing broadening, then make the carbonization of organic substance octylame be embedded in MoS by annealing in process
2between molecular layer, form superlattice structure; With common MoS
2(as nanometer sheet) is compared, and its advantage shows as good conductivity, interlamellar spacing broadening and not easily reunites;
2, simple, the reaction condition temperature of preparation method's technique of the present invention, with low cost;
3, end product of the present invention is not only based on laboratory basic research, can large-scale mass production;
4, the MoS for preparing of the present invention
2/ C superlattice heterojunction nanometer sheet self-assembled nanometer pipe has good application in energy storage, is particularly useful for as anode material of lithium-ion battery, 0.2 and 20.0Ag
-1under high current density, its discharge capacity is respectively up to 475 and 187mAhg
-1.At 1.0Ag
-1to circulate its discharge capacity after 200 times still up to 415mAhg under current density
-1, compared with second time discharge capacity, its capability retention is 107.8%.As can be seen here, MoS
2/ C superlattice heterojunction nanometer sheet self-assembled nanometer pipe has good embodiment in the application aspect of sodium-ion battery.
Accompanying drawing explanation
Fig. 1 is that the present invention is at preparation MoS
2the scanning electron microscope diagram of the different phase of/C superlattice heterojunction nanometer sheet self-assembled nanometer pipe;
Fig. 2 is the X-ray diffraction spectrogram that the sample of the embodiment of the present invention 2 preparation is annealed under different temperatures;
Fig. 3 is the MoS without annealing in process prepared by the embodiment of the present invention 1
2the scanning electron microscope diagram of nanometer sheet self-assembled nanometer pipe and transmission electron microscope figure;
Fig. 4 is the MoS after annealing in process prepared by the embodiment of the present invention 2
2the scanning electron microscope diagram of/C superlattice heterojunction nanometer sheet self-assembled nanometer pipe and transmission electron microscope figure;
Fig. 5 is the X-ray diffraction spectrogram of sample prepared by the embodiment of the present invention 1 and 2;
Fig. 6 is the Raman spectrogram of sample prepared by the embodiment of the present invention 1 and 2;
Fig. 7 is the thermogravimetric analysis figure of sample prepared by the embodiment of the present invention 1 and 2;
Fig. 8 is the cycle performance figure of the sodium-ion battery of sample prepared by the embodiment of the present invention 1 and 2.
Specific implementation method
Below in conjunction with specific embodiments and the drawings, the present invention will be further described, and be not restricted to scope of the present invention.
Embodiment 1
The present embodiment prepares nanotube as follows:
Take S1.2mmol, and join in 10mL octylame solution, stir 5 minutes under continuing to add 0.5mmol molybdenum source normal temperature, then add 15mL absolute ethyl alcohol, obtain mixed solution; Mixed solution is transferred in reactor and react 8 hours at 200 DEG C, obtain initial product; Initial product cleaning the most at last, then at 60 DEG C dry 12 hours; Products therefrom is designated as sample 1.
Embodiment 2
The present embodiment prepares nanotube as follows:
Take S1.2mmol, and join in 10mL octylame solution, stir 5 minutes under continuing to add 0.5mmol molybdenum source normal temperature, then add 15mL absolute ethyl alcohol, obtain mixed solution; Mixed solution is transferred in reactor and react 8 hours at 200 DEG C, obtain initial product; Initial product cleaning the most at last, then at 60 DEG C dry 12 hours;
To clean and dry after initial product under the protection of argon hydrogen, in 700 DEG C of annealing in process 1 hour, namely obtain MoS
2/ C heterojunction superlattice nanometer sheet self-assembled nanometer pipe, is designated as sample 2.
Comparative example 1 embodiment 2 is known, and difference is whether carried out annealing in process.
Fig. 3 is scanning electron microscopy (SEM) and transmission electron microscope (TEM) figure of embodiment 1 gained sample 1, wherein (a) and (b) figure are the scanning electron microscope diagram of sample 1 under different amplification respectively, therefrom can find out that its pattern is nanotube-shaped, diameter 250-300nm, length 3-6 μm, (c), (d), e () figure is the TEM figure done for further demonstrating product morphology feature, can find out that its tubular morphology is that many nanometer sheet assemble, and can find out that nanometer sheet has layer structure feature from high power transmission electron microscope (HRTEM) figure.
Fig. 4 is SEM and the TEM figure of embodiment 2 gained sample 2, wherein (a) and (b) figure are the SEM of sample 2 under different amplification respectively, therefrom can find out that its pattern is nanotube-shaped, compared to sample 1, length drops to about 1 μm, c () and (d) figure can find out that its nano tube structure is made up of nanometer sheet self assembly, wherein (e) figure is the HRTEM figure being selected from (c) figure, significantly can find out that nanometer sheet is by multilayer MoS
2molecular layer superposition is formed, adjacent MoS
2carbon-coating is embedded with, MoS between layer
2interlamellar spacing is 0.98nm, this and block MoS
2(002) interplanar distance (0.615nm) of material is compared, the remarkable broadening of spacing, and can find out adjacent MoS by (f) figure
2the spacing of molecular layer and carbon-coating is 0.49nm.Above-mentioned HRTEM figure shows MoS
2form sandwich structure between molecular layer and carbon-coating, form MoS
2/ C superlattice heterojunction.
Fig. 5 is the XRD figure of embodiment 1 and 2, and the curve (i) being wherein positioned at top is the X-ray diffraction peak of sample 1, and the curve (ii) of below is the X-ray diffraction peak of sample 2.Two broad peak 2 θ=33.3 of curve (i) ° and 56.9 ° of corresponding 2H-MoS of difference
2(JCPDF06-0097) (101) and (110) face.In addition, in 2 θ=4.50 there are three diffraction maximums in ° (d=1.960nm), 2 θ=8.96 ° (d=0.986nm) and ° (d=0.495nm) place, 2 θ=17.90; Wherein, the corresponding MoS of the diffraction maximum of 2 θ=8.96 ° (d=0.986nm)
2(002) crystal face, shows MoS
2interlamellar spacing by 0.615nm broadening to 0.986nm.Diffraction maximum correspondence (001) crystal face of 2 θ=4.5 °, shows at MoS
2intercalation reaction has octylame molecule.In curve (ii), a 2 θ=4.50 ° place diffraction maximum disappears, but the diffraction maximum of 2 θ=8.96 ° significantly strengthens, corresponding MoS
2(002) crystal face (d=0.986nm) of broadening; The corresponding adjacent MoS of diffraction maximum of 2 θ=17.90 °
2interlamellar spacing (d=0.495nm) between molecular layer and carbon atomic layer, proves to form MoS further
2/ C superlattice heterojunction.The diffraction maximum grow of sample 2, after showing annealing in process, the degree of crystallinity of material increases.
Fig. 6 is the Raman figure of embodiment 1 and 2, is wherein positioned at curve (i) counter sample 1 of top, curve (ii) counter sample 2 of below.Wherein, 402cm
-1the corresponding MoS in peak
2flat out-of-plane vibration A
1gpattern, 375cm
-1peak corresponding Mo-S key E
2gvibration mode, both MoS
2characteristic peak.Curve (i) is at 1200-1600cm
-1there is broad peak (D and G peak) to occur, show the product MoS of sample 1
2in atomic layer, octylame molecule does not have carbonization; In curve (ii), D band and G band become sharp-pointed, and after showing annealing, in sample 2, the degree of graphitization of carbon improves.
Fig. 7 is the thermogravimetric analysis figure of embodiment 1 and 2, is wherein positioned at curve (i) counter sample 1 of below, curve (ii) counter sample 2 of top.The content of C in sample 1 and sample 2 can be known by thermogravimetric analysis.Wherein calcine MoS in atmosphere
2become MoO
3the loss in weight 10%, is therefore about 12% from the content carbon the known sample 2 of curve (ii); Sample (1) has the obvious loss in weight caused by the volatilization of octylame molecule at 200-300 DEG C.If think MoS in sample 1 and sample 2
2the same with the mass ratio of carbon, so, as calculated, the octylame amount in sample 1 is about 21%.
For test sample chemical property, assemble sodium-ion battery testing as follows: work electrode to be mixed with the ratio of 60:20:20 by sample 1 or sample 2, carbon black and sodium carboxymethylcellulose to apply on Copper Foil, then 80 DEG C of dryings, to be stamped into diameter be in the disk of 16mm.Then by electrode discs at 110 DEG C vacuumize 4 hours and transfer to Ar protect gas glove box in assembled battery.Sodium metal sheet is to electrode, and electrolyte is NaClO
4solution (1.0molL
-1) and fluorinated ethylene carbonate (5%) assembling sodium-ion battery, its test is at room temperature carried out.
Fig. 8 is the cycle performance figure of the sodium-ion battery of sample 1 and sample 2, and analyze known from figure, current density is at 200mAg
-1time, the initial charge/discharge capacity of the electrode of the sample 2 of annealing is respectively up to 620mAhg
-1and 521mAhg
-1, its first coulombic efficiency reach 84%, this irreversible capacity loss is owing to defining SEI layer in cyclic process first.From second time circulation until 200 circulations, the MoS of annealing
2: C nano pipe charge/discharge capacity almost remains unchanged, at 200mAg
-1circulate 200 times under current density, reversible capacity is up to 477mAhg
-1.500 and 1000mAg
-1under current density, after 200 circulations, discharge capacity of the cell is respectively 475 and 415mAhg
-1, compared with their the 2nd discharge capacity, its capability retention is respectively 108.2% and 107.8%, thus indicates the MoS of annealing
2/ C nano pipe has excellent cyclical stability.
Claims (6)
1. a MoS
2/ C superlattice heterojunction nanometer sheet self-assembled nanometer pipe, is characterized in that: described nanotube is made up of nanometer sheet self assembly, and which floor MoS is described nanometer sheet be by
2molecular layer superposition is formed, adjacent MoS
2between molecular layer, intercalation has monolayer carbon atomic layer, forms MoS
2/ C superlattice heterojunction.
2. MoS according to claim 1
2/ C superlattice heterojunction nanometer sheet self-assembled nanometer pipe, is characterized in that: form MoS
2the adjacent MoS of nanometer sheet
2spacing between molecular layer is 0.98nm.
3. MoS according to claim 1
2/ C superlattice heterojunction nanometer sheet self-assembled nanometer pipe, is characterized in that: adjacent MoS in described superlattice heterojunction
2the interlamellar spacing of molecular layer and carbon atomic layer is 0.49nm.
4. the MoS described in a claim 1,2 or 3
2the preparation method of/C superlattice heterojunction nanometer sheet self-assembled nanometer pipe, is characterized in that carrying out as follows:
A, take S powder 1-2mmol, and join in 10-15mL octylame solution, continue to add 0.4-0.6mmol molybdenum source, stir 0-10 minute under normal temperature, then add 10-20mL anhydrous ethanol solvent, obtain mixed solution; Described mixed solution is transferred in reactor and at 170-200 DEG C, reacts 3-8 hour, obtain initial product;
B, by described initial product under the protection of argon hydrogen, 300-700 DEG C of annealing in process 1 hour, obtains target product.
5. preparation method according to claim 4, is characterized in that: described molybdenum source is ammonium molybdate or molybdenum trioxide.
6. the MoS described in a claim 1,2 or 3
2the application of/C superlattice heterojunction nanometer sheet self-assembled nanometer pipe, is characterized in that: for the negative material as sodium-ion battery.
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| CN110342474A (en) * | 2019-06-06 | 2019-10-18 | 中国科学技术大学 | A kind of two dimension high conductivity hydrogenation NbSe2Nano thin-film, preparation method and application |
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| CN106410136A (en) * | 2016-09-28 | 2017-02-15 | 辽宁石油化工大学 | Layered structure molybdenum disulfide/carbon composite material and preparation method and application thereof |
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| CN110544768B (en) * | 2019-08-13 | 2020-10-30 | 许昌学院 | Triangular tower conical Ni3S2.9Homogeneous superlattice thin film electrode material and preparation method and application thereof |
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| CN111293293A (en) * | 2020-02-19 | 2020-06-16 | 中国科学技术大学 | Molybdenum disulfide nanotube/sulfur composite cathode material with increased interlayer spacing and preparation method and application thereof |
| CN112259733A (en) * | 2020-10-21 | 2021-01-22 | 湘潭大学 | Nanotube-shaped magnesium ion battery positive electrode material and preparation method thereof |
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