CN106335925A - Method for preparing single-layer 2H phase molybdenum disulfide/graphene composite - Google Patents
Method for preparing single-layer 2H phase molybdenum disulfide/graphene composite Download PDFInfo
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- CN106335925A CN106335925A CN201610699082.2A CN201610699082A CN106335925A CN 106335925 A CN106335925 A CN 106335925A CN 201610699082 A CN201610699082 A CN 201610699082A CN 106335925 A CN106335925 A CN 106335925A
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- phase
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G39/00—Compounds of molybdenum
- C01G39/06—Sulfides
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/80—Particles consisting of a mixture of two or more inorganic phases
Abstract
The present invention discloses a method for preparing a single-layer 2H phase molybdenum disulfide/graphene composite, and specific steps are as follows: ammonium thiomolybdate and a lithium salt compound as raw materials can be synthesized into a lithium-intercalated 2H phase molybdenum sulfide block; 2H phase monolayer MoS2 nanosheets can be obtained by hydrolysis self-peeling of the lithium-intercalated 2H phase molybdenum sulfide block in water, and the single-layer 2H phase molybdenum disulfide/graphene composite can be obtained by self-assemble of the 2H phase monolayer MoS2 nanosheets and graphene oxide. The method has the advantages of being simple in process operation, mild in reaction condition, low in price of reagents, green and environmentally-friendly.
Description
Technical field
The invention belongs to the synthesis technical field of molybdenum bisuphide/graphene composite material is and in particular to one kind prepares individual layer
The method of 2h phase molybdenum bisuphide/graphene composite material.
Background technology
Molybdenum bisuphide has typical sandwich layer structure, due to the relatively weak Van der Waals force of its interlayer it is also possible to shell
From becoming the nanometer sheet of individual layer or few number of plies it is considered to be another considerable two-dimensional nano sheet material, there is uniqueness
Physics, chemically and electrically characteristic.Radisavljevic et al. test shows individual layer mos2Electrical conductivity than block mos2Improve
100 orders of magnitude are so that it has superior performance in electronic device and electronic sensor
(nat.nanotechnol.2011,6,147)；Mak et al. shows mos by calculating simulation2Peel off to individual layer from block, due to
Quantum confined effect, its energy gap is increased to the 1.8ev of direct band gap so that light induced electron is empty by the 1.3ev of indirect band gap
The separating power in cave improves (phys.rev.lett.2010,105)；Hinnemann et al. calculates nanometer by density letter formula
Level mos2The absorption hydrogen Gibbs free energy exposing active edge, find that there is very strong hydrogen adsorption capacity at its edge, and have
Metal pt equally close to the Hydrogen Evolution Performance of zero Gibbs free energy, thus being inferred to the mos of individual layer2Have more exposure activity
Edge, gets a good chance of becoming the catalyst (j.am.chem.soc.2005,127,5308) substituting pt as liberation of hydrogen material.chen
Et al. w.x. research shows, individual layer mos2With carbon-based material compound tense, have the capacity contribution (> 1500mah/g of superelevation), far
Exceed well over the theoretical value (j.mater.chem.2011,21,6251) of its block materials.
There is three kinds of phases, i.e. 1t, 2h and 3r phase in molybdenum bisuphide.Wherein, 1t phase is mos2With a s-mo-s unimolecule
Layer is as minimum repetitive stacking, and 2h with 3r phase is using two and three s-mo-s monolayers as minimum repetitive
Stacking.Most of mos in nature2It is to be existed with 2h stable phase, 1t with 3r phase belongs to metastable structure, under certain condition
2h phase can be changed into.Mos due to individual layer 2h phase2Have been out the characteristic that bilayer is minimum repetitive, therefore
Also referred to as 1h phase.The mos of different phase2The physicochemical characteristics that material is presented also is not quite similar.For example, 2h state mos2Material
Material shows the characteristic of semiconductor that energy gap is 1.3-1.9ev, and it is by how many sizes to adjust energy gap of the number of plies；
And the mos of 1t state2Material then presents metallic character, and its superior electric conductivity is led in catalytic water decomposing hydrogen-production and super capacitor
Domain achieve important breakthrough (advanced energy materials, 2016, doi:10.1002/
Aenm.201502555).
Although individual layer mos2Nano material is in heat, the property of the aspect such as electricity, light, mechanics and its in field of optoelectronic devices
Potential application causes the extensive concern of scientific research personnel.However, general chemistry, Physical are difficult to prepare pure single layer structure
mos2The individual layer molybdenum sulfide of nano material, especially different phase peels off preparation.Prepare individual layer mos at present2Nano material main
There are micromechanical forces stripping method, chemical vapour deposition technique, lithium ion graft process and liquid phase ultrasonic method etc., these stripping means are not only
Complex operation, complex process, and individual layer mos2Yield extremely low, major part is few number of stories m os that thickness is 1-100nm2Nanometer
Piece, rather than individual layer mos truly2.Prepare individual layer mos except being difficult to expeditiously stripping2Outside nanometer sheet, mos2Nanometer
Piece can only be peeled off in the high boiling organic solvent such as dimethylformamide and n- methyl pyrrolidone and preserve, and these have
Machine solvent viscosity is big, boiling point is very high, during being collected by centrifugation, individual layer or less number of stories m os2It is gathered into multilayer mos again2Receive
Rice piece, thus limit individual layer mos2Nanometer sheet is in the exploration of some scientific researches or industrial circle and application.Additionally, mos2Nanometer sheet
During real application research, often it is combined with the material with carbon element such as agraphitic carbon, CNT, carbon fiber and Graphene, to increase
Plus its electric conductivity.
Content of the invention
Present invention solves the technical problem that there is provided a kind of preparation of simple, safe efficient and suitable large-scale production
The method of individual layer 2h phase molybdenum bisuphide/graphene composite material, the method is with ammonium thiomolybdate and lithium salt compound as raw material,
It is thermally treated resulting in the slotting lithium li of 2h phase at a certain temperature2mos2Block, slotting lithium li2mos2Block hydrolyzes certainly in deionized water
Row is peeled off, then is self-assembled into individual layer 2h phase molybdenum bisuphide/graphene composite material with the graphene oxide adding, prepared individual layer
2h phase molybdenum bisuphide/graphene composite material both can improve the electric conductivity of material, can effectively suppress individual layer 2h phase two again
The reunion of molybdenum sulfide.
The present invention is that solution above-mentioned technical problem adopts the following technical scheme that, one kind prepares individual layer 2h phase molybdenum bisuphide/stone
The method of black alkene composite is it is characterised in that concretely comprise the following steps:
(1) ammonium thiomolybdate and lithium salt compound are pressed 1:2 mixed in molar ratio to grind, the mixture after grinding is protected in inert gas
It is incubated 1-10h in 200-400 DEG C under shield, be cooled to room temperature and obtain inserting the 2h phase molybdenum sulfide block of lithium；
(2) the 2h phase molybdenum sulfide block of slotting lithium is placed directly within deionized water, 5-30min is peeled off in assisting ultrasonic hydrolysis, then will
The suspension obtaining is placed in a centrifuge, and obtains individual layer 2h phase mos after being centrifuged removing unstripped sediment2Nanometer sheet
Suspension；
(3) add graphene oxide into individual layer 2h phase mos2In nanometer sheet suspension, ultrasonic disperse 5-10min, it is subsequently adding
Hydrazine hydrate continues ultrasonic 0.5-2h and obtains individual layer 2h phase mos2/ graphene suspension；
(4) by the individual layer obtaining 2h phase mos2/ graphene suspension uses water and ethanol centrifuge washing to remove on centrifuge respectively
Soluble impurity, finally sediment individual layer 2h phase molybdenum bisuphide/graphene composite material is scattered in small molecule solvent and preserves,
Wherein individual layer 2h phase mos2The thickness of nanometer sheet is less than 1nm.
Limit further, the lithium salt compound described in step (1) be lithium hydroxide, lithium chloride, lithium acetate, lithium carbonate,
One or more of lithium sulfate or lithium nitrate.
Limit further, the centrifuge speed described in step (2) is 1000r/min, the centrifuge described in step (4)
Rotating speed is 4000-20000r/min.
Limit further, the graphene oxide described in step (3) and individual layer 2h phase mos2Mos in nanometer sheet suspension2's
Mass ratio is 0.005-0.2:1.
Limit further, the small molecule solvent described in step (4) be water, methyl alcohol, ethanol, isopropanol, butanol, acetone,
N- methyl pyrrolidone or n- NMF.
The present invention compared with prior art has the advantage that
1st, the present invention, with ammonium thiomolybdate and lithium salt compound as raw material, can synthesize slotting lithium by simple temperature control
2h phase molybdenum sulfide block, the 2h phase molybdenum sulfide block of slotting lithium can hydrolyze in water voluntarily peels off into 2h phase individual layer mos2Nanometer
Piece, then it is self-assembly of individual layer 2h phase molybdenum bisuphide/graphene composite material with graphene oxide, and can be in water, ethanol
Deng stable existence in small molecule solvent；
2nd, the 2h phase individual layer mos that the present invention obtains2The thickness of nanometer sheet is less than 1nm, rather than 1-100nm thickness of the prior art
Mos2Nanometer sheet；
3rd, the present invention synthesis individual layer 2h phase molybdenum bisuphide/graphene composite material can be used for individual layer molybdenum sulfide light liberation of hydrogen,
The research in the field such as electro-catalysis and energy storage；
4th, present invention process is simple to operate, and reaction condition is gentle, and agents useful for same is cheap, environmental protection.
Specific embodiment
By the following examples the above of the present invention is described in further details, but this should not be interpreted as this
The scope inventing above-mentioned theme is only limitted to below example, all belongs to this based on the technology that the above of the present invention is realized
Bright scope.
Embodiment 1
Weigh the lithium hydroxide of 0.008mol and the ammonium thiomolybdate of 0.004mol respectively, mixed grinding 1h in agate mortar,
Mixture after grinding is placed in corundum crucible, is placed in tube furnace, logical argon gas protection, temperature programming, to 400 DEG C, is incubated
1h, then proceedes to logical argon gas and is naturally cooling to room temperature, obtain inserting the 2h phase molybdenum sulfide (li of lithium2mos4) block；Sulfuration by slotting lithium
Molybdenum block is placed in the container filling 100ml deionized water, ultrasonic disperse 10min, and the suspension after dispersion in rotating speed is
Centrifugation precipitation on the centrifuge of 1000r/min；Molybdenum disulfide content addition 1 according to removing in precipitation rear suspension liquid:
The graphene oxide of 0.005 mass ratio, adds the hydrazine hydrate that 0.5ml mass fraction is 80% after ultrasonic disperse 10min, continue super
Sound 0.5h obtains individual layer 2h phase mos2/ graphene suspension；By the individual layer obtaining 2h phase mos2/ graphene suspension in rotating speed is
Water and 3 removal soluble impurities of ethanol centrifuge washing are used on the centrifuge of 4000r/min, finally by sediment individual layer 2h respectively
Phase molybdenum bisuphide/graphene composite material is scattered in 200ml deionized water and preserves.The individual layer 2h phase molybdenum bisuphide/stone of gained
In black alkene composite, the content of Graphene is about 0.25%.
Embodiment 2
Weigh the lithium acetate of 0.008mol and the ammonium thiomolybdate of 0.004mol, mixed grinding 1h in agate mortar respectively, incite somebody to action
Mixture after grinding is placed in corundum crucible, is placed in tube furnace, logical argon gas protection, and temperature programming, to 200 DEG C, is incubated
10h, then proceedes to logical argon gas and is naturally cooling to room temperature, obtain inserting the 2h phase molybdenum sulfide (li of lithium2mos4) block；Sulphur by slotting lithium
Change molybdenum block to be placed in the container filling 200ml deionized water, ultrasonic disperse 10min, the suspension after dispersion in rotating speed is
Centrifugation precipitation on the centrifuge of 1000r/min；Molybdenum disulfide content addition 1 according to removing in precipitation rear suspension liquid:
The graphene oxide of 0.01 mass ratio, adds the hydrazine hydrate that 1ml mass fraction is 80%, continues ultrasonic after ultrasonic disperse 10min
0.5h obtains individual layer 2h phase mos2/ graphene suspension；By the individual layer obtaining 2h phase mos2/ graphene suspension in rotating speed is
Water and 3 removal soluble impurities of ethanol centrifuge washing are used on the centrifuge of 10000r/min, finally by sediment individual layer respectively
2h phase molybdenum bisuphide/graphene composite material is scattered in 200ml absolute ethyl alcohol and preserves.The individual layer 2h phase molybdenum bisuphide of gained/
In graphene composite material, the content of Graphene is about 0.5%.
Embodiment 3
Weigh the lithium nitrate of 0.008mol and the ammonium thiomolybdate of 0.004mol, mixed grinding 1h in agate mortar respectively, incite somebody to action
Mixture after grinding is placed in corundum crucible, is placed in tube furnace, logical argon gas protection, and temperature programming, to 300 DEG C, is incubated
5h, then proceedes to logical argon gas and is naturally cooling to room temperature, obtain inserting the 2h phase molybdenum sulfide (li of lithium2mos4) block；Sulfuration by slotting lithium
Molybdenum block is placed in the container filling 100ml deionized water, ultrasonic disperse 5min, and the suspension after dispersion is 1000r/ in rotating speed
Centrifugation precipitation on the centrifuge of min；Add 1:0.10 mass according to removing the molybdenum disulfide content in precipitation rear suspension liquid
The graphene oxide of ratio, adds the hydrazine hydrate that 5ml mass fraction is 80% after ultrasonic disperse 10min, continue ultrasonic 1h and obtain individual layer
2h phase mos2/ graphene suspension；By the individual layer obtaining 2h phase mos2/ graphene suspension rotating speed for 15000r/min from
Water and 3 removal soluble impurities of ethanol centrifuge washing are used on scheming, finally by sediment individual layer 2h phase molybdenum bisuphide/stone respectively
Black alkene composite is scattered in 200ml isopropanol and preserves.Stone in the individual layer 2h phase molybdenum bisuphide/graphene composite material of gained
The content of black alkene is about 5%.
Embodiment 4
Weigh the lithium carbonate of 0.008mol and the ammonium thiomolybdate of 0.004mol, mixed grinding 1h in agate mortar respectively, grind
Mixture being placed in corundum crucible after mill, is placed in tube furnace, logical argon gas protection, and temperature programming, to 300 DEG C, is incubated
5h, then proceedes to logical argon gas and is naturally cooling to room temperature, obtain inserting the 2h phase molybdenum sulfide (li of lithium2mos4) block；Sulfuration by slotting lithium
Molybdenum block is placed in the container filling 100ml deionized water, ultrasonic disperse 30min, and the suspension after dispersion in rotating speed is
Centrifugation precipitation on the centrifuge of 1000r/min；Add 1:0.2 according to removing the molybdenum disulfide content in precipitation rear suspension liquid
The graphene oxide of mass ratio, adds the hydrazine hydrate that 10ml mass fraction is 80% after ultrasonic disperse 10min, continue ultrasonic 2h and obtain
To individual layer 2h phase mos2/ graphene suspension；By the individual layer obtaining 2h phase mos2/ graphene suspension is 20000r/ in rotating speed
Water and 3 removal soluble impurities of ethanol centrifuge washing are used on the centrifuge of min, finally by sediment individual layer 2h phase two sulphur respectively
Change molybdenum/graphene composite material and be scattered in preservation in 200ml n- methyl pyrrolidone.The individual layer 2h phase molybdenum bisuphide/stone of gained
In black alkene composite, the content of Graphene is about 5%.
Embodiment above describes general principle, principal character and the advantage of the present invention, the technical staff of the industry should
Understand, the present invention is not restricted to the described embodiments, the simply explanation present invention's described in above-described embodiment and specification is former
Reason, under the scope without departing from the principle of the invention, the present invention also has various changes and modifications, and these changes and improvements each fall within
In the scope of protection of the invention.
Claims (5)
1. a kind of method preparing individual layer 2h phase molybdenum bisuphide/graphene composite material is it is characterised in that concretely comprise the following steps:
(1) ammonium thiomolybdate and lithium salt compound are pressed 1:2 mixed in molar ratio to grind, the mixture after grinding is protected in inert gas
It is incubated 1-10h in 200-400 DEG C under shield, be cooled to room temperature and obtain inserting the 2h phase molybdenum sulfide block of lithium；
(2) the 2h phase molybdenum sulfide block of slotting lithium is placed directly within deionized water, 5-30min is peeled off in assisting ultrasonic hydrolysis, then will
The suspension obtaining is placed in a centrifuge, and obtains individual layer 2h phase mos after being centrifuged removing unstripped sediment2Nanometer sheet
Suspension；
(3) add graphene oxide into individual layer 2h phase mos2In nanometer sheet suspension, ultrasonic disperse 5-10min, it is subsequently adding water
Close the hydrazine ultrasonic 0.5-2h of continuation and obtain individual layer 2h phase mos2/ graphene suspension；
(4) by the individual layer obtaining 2h phase mos2/ graphene suspension is removed with water and ethanol centrifuge washing on centrifuge respectively can
Solubility impurity, finally sediment individual layer 2h phase molybdenum bisuphide/graphene composite material is scattered in small molecule solvent and preserves, its
Middle individual layer 2h phase mos2The thickness of nanometer sheet is less than 1nm.
2. the method preparing individual layer 2h phase molybdenum bisuphide/graphene composite material according to claim 1, its feature exists
In: the lithium salt compound described in step (1) is in lithium hydroxide, lithium chloride, lithium acetate, lithium carbonate, lithium sulfate or lithium nitrate
One or more.
3. the method preparing individual layer 2h phase molybdenum bisuphide/graphene composite material according to claim 1, its feature exists
In: the centrifuge speed described in step (2) is 1000r/min, and the centrifuge speed described in step (4) is 4000-
20000r/min.
4. the method preparing individual layer 2h phase molybdenum bisuphide/graphene composite material according to claim 1, its feature exists
In: the graphene oxide described in step (3) and individual layer 2h phase mos2Mos in nanometer sheet suspension2Mass ratio be 0.005-
0.2:1.
5. the method preparing individual layer 2h phase molybdenum bisuphide/graphene composite material according to claim 1, its feature exists
In: the small molecule solvent described in step (4) be water, methyl alcohol, ethanol, isopropanol, butanol, acetone, n- methyl pyrrolidone or
N- NMF.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106987857A (en) * | 2017-03-09 | 2017-07-28 | 陕西科技大学 | Single-layer metal structure molybdenum disulfide/redox graphene complex and preparation method thereof |
| CN108893755A (en) * | 2018-07-09 | 2018-11-27 | 南京师范大学 | Mixing removing one-step method prepares the method and its application of nano-scale molybdenum disulfide and graphene complex |
| CN109183058A (en) * | 2018-09-12 | 2019-01-11 | 电子科技大学 | A kind of construction method of the catalytic hydrogen evolution electrode of abundant exposed molybdenum disulfide active sites |
| CN111569911A (en) * | 2020-05-22 | 2020-08-25 | 重庆工商大学 | Preparation method of 3R type molybdenum disulfide catalyst |
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| CN102701192A (en) * | 2012-06-08 | 2012-10-03 | 浙江大学 | Method for preparing monolayer MoS2 and graphene compounded nano material |
| CN104310482A (en) * | 2014-09-29 | 2015-01-28 | 南京邮电大学 | Method for preparing molybdenum disulfide nanosheets by ultrasonic-assisted chemical intercalation |
| WO2016042309A1 (en) * | 2014-09-18 | 2016-03-24 | The University Of Manchester | Proton conducting membrane comprising monolithic 2d material and ionomer, a process for preparing same and use of same in fuel cell and hydrogen gas sensor |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106987857A (en) * | 2017-03-09 | 2017-07-28 | 陕西科技大学 | Single-layer metal structure molybdenum disulfide/redox graphene complex and preparation method thereof |
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| CN108893755A (en) * | 2018-07-09 | 2018-11-27 | 南京师范大学 | Mixing removing one-step method prepares the method and its application of nano-scale molybdenum disulfide and graphene complex |
| CN109183058A (en) * | 2018-09-12 | 2019-01-11 | 电子科技大学 | A kind of construction method of the catalytic hydrogen evolution electrode of abundant exposed molybdenum disulfide active sites |
| CN109183058B (en) * | 2018-09-12 | 2020-08-18 | 电子科技大学 | Construction method of catalytic hydrogen evolution electrode capable of fully exposing molybdenum disulfide active site |
| CN111569911A (en) * | 2020-05-22 | 2020-08-25 | 重庆工商大学 | Preparation method of 3R type molybdenum disulfide catalyst |
| CN111569911B (en) * | 2020-05-22 | 2022-04-22 | 重庆工商大学 | Preparation method of 3R type molybdenum disulfide catalyst |
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