CN106335925B - A kind of method for preparing individual layer 2H phases molybdenum disulfide/graphene composite material - Google Patents
A kind of method for preparing individual layer 2H phases molybdenum disulfide/graphene composite material Download PDFInfo
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- CN106335925B CN106335925B CN201610699082.2A CN201610699082A CN106335925B CN 106335925 B CN106335925 B CN 106335925B CN 201610699082 A CN201610699082 A CN 201610699082A CN 106335925 B CN106335925 B CN 106335925B
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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
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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 invention discloses a kind of method for preparing individual layer 2H phases molybdenum disulfide/graphene composite material, detailed process is：Using ammonium thiomolybdate and lithium salt compound as raw material, the 2H phase molybdenum sulfide blocks of slotting lithium can be synthesized by simple temperature control, the 2H phase molybdenum sulfides block of slotting lithium can be hydrolyzed in water voluntarily peels off into 2H phase individual layers MoS2Nanometer sheet, then it is self-assembly of individual layer 2H phases molybdenum disulfide/graphene composite material with graphene oxide.Present invention process is simple to operate, and reaction condition is gentle, and agents useful for same is cheap, environmental protection.
Description
Technical field
The invention belongs to the synthesis technical field of molybdenum disulfide/graphene composite material, and in particular to one kind prepares individual layer
The method of 2H phases molybdenum disulfide/graphene composite material.
Background technology
Molybdenum disulfide has typical sandwich layer structure, due to the relatively weak Van der Waals force of its interlayer, can also shell
From the nanometer sheet into individual layer or few number of plies, it is considered to be another considerable two-dimensional nano sheet material, with uniqueness
Physics, chemically and electrically characteristic.Radisavljevic et al. tests show individual layer MoS2Electrical conductivity than block MoS2Improve
100 orders of magnitude so that it has superior performance in electronic device and electronic sensor
（Nat.Nanotechnol.2011,6,147）；Mak et al. shows MoS by calculating simulation2Peeled off from block to individual layer, due to
Quantum confined effect, its energy gap is increased to the 1.8eV of direct band gap by the 1.3eV of indirect band gap so that light induced electron is empty
The separating capacity in cave is improved（Phys.Rev.Lett.2010,105）；Hinnemann et al. calculates nanometer by density letter formula
Level MoS2The active edge of exposure absorption hydrogen Gibbs free energy, it is found that there is very strong hydrogen adsorption capacity at its edge, and have
Pt metal is equally close to the Hydrogen Evolution Performance of zero Gibbs free energy, so as to be inferred to the MoS of individual layer2Possess more exposure activity
Edge, gets a good chance of turning into the catalyst for substituting Pt as liberation of hydrogen material（J.Am.Chem.Soc.2005,127,5308）.Chen
Et al. W.X. research shows, individual layer MoS2With carbon-based material compound tense, have the capacity contribution of superelevation（>1500mAh/g）, far
Exceed well over the theoretical value of its block materials（J.Mater.Chem.2011,21,6251）.
There are three kinds of phases, i.e. 1T, 2H and 3R phase in molybdenum disulfide.Wherein, 1T phases are MoS2With a S-Mo-S unimolecule
Layer is stacked as minimum repeat unit, and 2H with 3R phases are to be used as minimum repeat unit using two and three S-Mo-S monolayers
Stack.Major part MoS in nature2It is to exist with 2H stable phases, 1T with 3R phases belong to metastable structure, under certain condition
2H phases can be changed into.Due to the MoS of individual layer 2H phases2The characteristic that bilayer is minimum repeat unit is lost, therefore
Also referred to as 1H phases.The MoS of different phase2The physicochemical characteristics that material is presented also is not quite similar.For example, 2H states MoS2Material
Material shows the characteristic of semiconductor that energy gap is 1.3-1.9eV, its by the number of plies number adjust the size of energy gap；
And the MoS of 1T states2Material then shows metallic character, and its superior electric conductivity is led in catalytic water decomposing hydrogen-production and super capacitor
Domain achieves important breakthrough（Advanced Energy Materials,2016,DOI:10.1002/
aenm.201502555）.
Although individual layer MoS2Property of the nano material in terms of heat, 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, which is peeled off, to be prepared.Prepare individual layer MoS at present2Nano material it is 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
It is cumbersome, complex process, and individual layer MoS2Yield it is extremely low, be largely thickness be 1-100nm few number of plies MoS2Nanometer
Piece, rather than individual layer MoS truly2.Individual layer MoS is prepared except being difficult to expeditiously stripping2Outside nanometer sheet, MoS2Nanometer
Piece can only be peeled off and preserved in the high boiling organic solvent such as dimethylformamide and 1-METHYLPYRROLIDONE, and these have
Machine solvent viscosity is big, boiling point is very high, during being collected by centrifugation, individual layer or few number of plies MoS2Multilayer MoS is gathered into again2Receive
Rice piece, so as to limit individual layer MoS2Nanometer sheet is in some scientific researches or the exploration of industrial circle and application.In addition, MoS2Nanometer sheet
During real application research, often it is combined with the carbon material such as agraphitic carbon, CNT, carbon fiber and graphene, to increase
Plus its electric conductivity.
The 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 phases molybdenum disulfide/graphene composite material, this method be using ammonium thiomolybdate and lithium salt compound as raw material,
The slotting lithium Li of 2H phases is thermally treated resulting at a certain temperature2MoS2Block, inserts lithium Li2MoS2Block is hydrolyzed certainly in deionized water
Row is peeled off, then is self-assembled into individual layer 2H phases molybdenum disulfide/graphene composite material, obtained individual layer with the graphene oxide of addition
2H phases molybdenum disulfide/graphene composite material can both improve the electric conductivity of material, can effectively suppress individual layer 2H phases two again
The reunion of molybdenum sulfide.
Wei Xie Decision above-mentioned technical problems of the present invention adopt the following technical scheme that one kind prepares individual layer 2H phases molybdenum disulfide/stone
The method of black alkene composite, 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 are ground, and the mixture after grinding is in indifferent gas
1-10h is incubated in 200-400 DEG C under body protection, the 2H phase molybdenum sulfide blocks that room temperature obtains inserting lithium are cooled to；
（2）The 2H phase molybdenum sulfide blocks of slotting lithium are placed directly within deionized water, 5-30min is peeled off in assisting ultrasonic hydrolysis,
Obtained suspension is placed in a centrifuge again, is centrifuged obtaining individual layer 2H phases MoS after removing unstripped sediment2Receive
Rice piece suspension；
（3）Add graphene oxide into individual layer 2H phases MoS2In nanometer sheet suspension, ultrasonic disperse 5-10min, then
Add hydrazine hydrate continuation ultrasound 0.5-2h and obtain individual layer 2H phases MoS2/ graphene suspension；
（4）By obtained individual layer 2H phases MoS2/ graphene suspension uses water and ethanol centrifuge washing respectively on centrifuge
Soluble impurity is removed, finally sediment individual layer 2H phases molybdenum disulfide/graphene composite material is scattered in small molecule solvent
Preserve, wherein individual layer 2H phases MoS2The thickness of nanometer sheet is less than 1nm.
Further limit, step（1）Described in lithium salt compound for lithium hydroxide, lithium chloride, lithium acetate, lithium carbonate,
One or more in lithium sulfate or lithium nitrate.
Further limit, step（2）Described in centrifuge speed be 1000r/min, step（4）Described in centrifuge
Rotating speed is 4000-20000r/min.
Further limit, step（3）Described in graphene oxide and individual layer 2H phases MoS2MoS in nanometer sheet suspension2's
Mass ratio is 0.005-0.2:1.
Further limit, step（4）Described in small molecule solvent for water, methanol, ethanol, isopropanol, butanol, acetone,
1-METHYLPYRROLIDONE or N-METHYLFORMAMIDE.
The present invention has advantages below compared with prior art：
1st, the present invention can be synthesized slotting using ammonium thiomolybdate and lithium salt compound as raw material by simple temperature control
The 2H phase molybdenum sulfide blocks of lithium, the 2H phase molybdenum sulfides block of slotting lithium can be hydrolyzed in water voluntarily peels off into 2H phase individual layers MoS2Receive
Rice piece, then individual layer 2H phases molybdenum disulfide/graphene composite material is self-assembly of with graphene oxide, and can be in water, second
It is stabilized in the small molecule solvents such as alcohol；
2nd, the 2H phase individual layers MoS that the present invention is obtained2The thickness of nanometer sheet is less than 1nm, rather than 1-100nm of the prior art
The MoS of thickness2Nanometer sheet；
3rd, individual layer 2H phases molybdenum disulfide/graphene composite material that the present invention is synthesized can be used for individual layer molybdenum sulfide in light analysis
The research in the fields such as hydrogen, 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.
Embodiment
The above to the present invention is described in further details by the following examples, but this should not be interpreted as to this
The scope for inventing above-mentioned theme is only limitted to following embodiment, and all technologies realized based on the above of the present invention belong to this hair
Bright scope.
Embodiment 1
0.008mol lithium hydroxide and 0.004mol ammonium thiomolybdate are weighed respectively, the mixed grinding in agate mortar
1h, the mixture after grinding is placed in corundum crucible, is placed in tube furnace, lead to argon gas protection, temperature programming to 400 DEG C,
1h is incubated, logical argon gas is then proceeded to and is naturally cooling to room temperature, obtain inserting the 2H phase molybdenum sulfides of lithium（Li2MoS4）Block；By slotting lithium
Molybdenum sulfide block is placed in the container for filling 100mL deionized waters, ultrasonic disperse 10min, and the suspension after disperseing is in rotating speed
Precipitation is centrifuged on 1000r/min centrifuge；Molybdenum disulfide content according to removing in precipitation rear suspension liquid adds 1:
The hydrazine hydrate that 0.5mL mass fractions are 80% is added after the graphene oxide of 0.005 mass ratio, ultrasonic disperse 10min, continues super
Sound 0.5h obtains individual layer 2H phases MoS2/ graphene suspension；By obtained individual layer 2H phases MoS2/ graphene suspension is in rotating speed
Respectively with 3 removal soluble impurities of water and ethanol centrifuge washing on 4000r/min centrifuge, finally by sediment individual layer 2H
Phase molybdenum disulfide/graphene composite material, which is scattered in 200mL deionized waters, to be preserved.Individual layer 2H phases molybdenum disulfide/stone of gained
The content of graphene is about 0.25% in black alkene composite.
Embodiment 2
0.008mol lithium acetate and 0.004mol ammonium thiomolybdate are weighed respectively, the mixed grinding in agate mortar
1h, the mixture after grinding is placed in corundum crucible, is placed in tube furnace, lead to argon gas protection, temperature programming to 200 DEG C,
10h is incubated, logical argon gas is then proceeded to and is naturally cooling to room temperature, obtain inserting the 2H phase molybdenum sulfides of lithium（Li2MoS4）Block；By slotting lithium
Molybdenum sulfide block be placed in the container for filling 200mL deionized waters, ultrasonic disperse 10min, disperse after suspension in rotating speed
To centrifuge precipitation on 1000r/min centrifuge；Molybdenum disulfide content according to removing in precipitation rear suspension liquid adds 1:
The hydrazine hydrate that 1mL mass fractions are 80% is added after the graphene oxide of 0.01 mass ratio, ultrasonic disperse 10min, continues ultrasound
0.5h obtains individual layer 2H phases MoS2/ graphene suspension；By obtained individual layer 2H phases MoS2/ graphene suspension is in rotating speed
Respectively with 3 removal soluble impurities of water and ethanol centrifuge washing on 10000r/min centrifuge, finally by sediment individual layer
2H phases molybdenum disulfide/graphene composite material, which is scattered in 200mL absolute ethyl alcohols, to be preserved.The individual layer 2H phases molybdenum disulfide of gained/
The content of graphene is about 0.5% in graphene composite material.
Embodiment 3
0.008mol lithium nitrate and 0.004mol ammonium thiomolybdate are weighed respectively, the mixed grinding in agate mortar
1h, the mixture after grinding is placed in corundum crucible, is placed in tube furnace, lead to argon gas protection, temperature programming to 300 DEG C,
5h is incubated, logical argon gas is then proceeded to and is naturally cooling to room temperature, obtain inserting the 2H phase molybdenum sulfides of lithium（Li2MoS4）Block；By slotting lithium
Molybdenum sulfide block is placed in the container for filling 100mL deionized waters, ultrasonic disperse 5min, and the suspension after disperseing is in rotating speed
Precipitation is centrifuged on 1000r/min centrifuge；Molybdenum disulfide content according to removing in precipitation rear suspension liquid adds 1:
The hydrazine hydrate that 5mL mass fractions are 80% is added after the graphene oxide of 0.10 mass ratio, ultrasonic disperse 10min, continues ultrasound 1h
Obtain individual layer 2H phases MoS2/ graphene suspension；By obtained individual layer 2H phases MoS2/ graphene suspension is 15000r/ in rotating speed
Respectively with 3 removal soluble impurities of water and ethanol centrifuge washing on min centrifuge, finally by the sulphur of sediment individual layer 2H phases two
Change molybdenum/graphene composite material and be scattered in preservation in 200mL isopropanols.Individual layer 2H phases molybdenum disulfide/graphene of gained is combined
The content of graphene is about 5% in material.
Embodiment 4
0.008mol lithium carbonate and 0.004mol ammonium thiomolybdate are weighed respectively, the mixed grinding in agate mortar
1h, mixture is placed in corundum crucible after grinding, is placed in tube furnace, lead to argon gas protection, temperature programming to 300 DEG C,
5h is incubated, logical argon gas is then proceeded to and is naturally cooling to room temperature, obtain inserting the 2H phase molybdenum sulfides of lithium（Li2MoS4）Block；By slotting lithium
Molybdenum sulfide block is placed in the container for filling 100mL deionized waters, ultrasonic disperse 30min, and the suspension after disperseing is in rotating speed
Precipitation is centrifuged on 1000r/min centrifuge；Molybdenum disulfide content according to removing in precipitation rear suspension liquid adds 1:0.2
The hydrazine hydrate that 10mL mass fractions are 80% is added after the graphene oxide of mass ratio, ultrasonic disperse 10min, continues ultrasound 2h and obtains
To individual layer 2H phases MoS2/ graphene suspension；By obtained individual layer 2H phases MoS2/ graphene suspension is 20000r/ in rotating speed
Respectively with 3 removal soluble impurities of water and ethanol centrifuge washing on min centrifuge, finally by the sulphur of sediment individual layer 2H phases two
Change molybdenum/graphene composite material and be scattered in preservation in 200mL 1-METHYLPYRROLIDONEs.Individual layer 2H phases molybdenum disulfide/stone of gained
The content of graphene is about 5% in black alkene composite.
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 limited to the above embodiments, the original for simply illustrating the present invention described in above-described embodiment and specification
Reason, under the scope for not departing from the principle of the invention, various changes and modifications of the present invention are possible, and these changes and improvements are each fallen within
In the scope of protection of the invention.
Claims (5)
1. a kind of method for preparing individual layer 2H phases molybdenum disulfide/graphene composite material, 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 are ground, and the mixture after grinding is protected in inert gas
1-10h is incubated in 200-400 DEG C under shield, the 2H phase molybdenum sulfide blocks that room temperature obtains inserting lithium are cooled to；
（2）The 2H phase molybdenum sulfide blocks of slotting lithium are placed directly within deionized water, 5-30min is peeled off in assisting ultrasonic hydrolysis, then will
Obtained suspension is placed in a centrifuge, and is centrifuged obtaining individual layer 2H phases MoS after removing unstripped sediment2Nanometer sheet
Suspension；
（3）Add graphene oxide into individual layer 2H phases MoS2In nanometer sheet suspension, then ultrasonic disperse 5-10min adds water
Close hydrazine continuation ultrasound 0.5-2h and obtain individual layer 2H phases MoS2/ graphene suspension；
（4）By obtained individual layer 2H phases MoS2/ graphene suspension is removed with water and ethanol centrifuge washing respectively on centrifuge can
Sediment individual layer 2H phases molybdenum disulfide/graphene composite material, is finally scattered in small molecule solvent and preserves by solubility impurity, its
Middle individual layer 2H phases MoS2The thickness of nanometer sheet is less than 1nm.
2. the method according to claim 1 for preparing individual layer 2H phases molybdenum disulfide/graphene composite material, its feature exists
In：Step（1）Described in lithium salt compound be lithium chloride, lithium acetate, lithium carbonate, lithium sulfate or lithium nitrate in one kind or many
Kind.
3. the method according to claim 1 for preparing individual layer 2H phases molybdenum disulfide/graphene composite material, its feature exists
In：Step（2）Described in centrifuge speed be 1000r/min, step（4）Described in centrifuge speed be 4000-
20000r/min。
4. the method according to claim 1 for preparing individual layer 2H phases molybdenum disulfide/graphene composite material, its feature exists
In：Step（3）Described in graphene oxide and individual layer 2H phases MoS2MoS in nanometer sheet suspension2Mass ratio be 0.005-
0.2:1。
5. the method according to claim 1 for preparing individual layer 2H phases molybdenum disulfide/graphene composite material, its feature exists
In：Step（4）Described in small molecule solvent for water, methanol, ethanol, isopropanol, butanol, acetone, 1-METHYLPYRROLIDONE or
N-METHYLFORMAMIDE.
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| CN106987857B (en) * | 2017-03-09 | 2018-12-25 | 陕西科技大学 | Single-layer metal structure molybdenum disulfide/redox graphene complex and preparation method thereof |
| CN108893755B (en) * | 2018-07-09 | 2020-08-25 | 南京师范大学 | Method for preparing nano-sized molybdenum disulfide and graphene compound by mixed stripping one-step method and application thereof |
| 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 |
| 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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| CN102683647B (en) * | 2012-06-08 | 2015-06-03 | 浙江大学 | Preparation method of graphene-like MoS2/graphene combined electrode of lithium ion battery |
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