CN106257609A - A kind of method preparing monolayer 1T phase molybdenum bisuphide/graphene composite material - Google Patents
A kind of method preparing monolayer 1T phase molybdenum bisuphide/graphene composite material Download PDFInfo
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
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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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- 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 discloses a kind of method preparing monolayer 1T phase molybdenum bisuphide/graphene composite material, detailed process is: with ammonium thiomolybdate and lithium salt compound as raw material, control to synthesize the 1T phase molybdenum sulfide block of slotting lithium by simple temperature, the 1T phase molybdenum sulfide block of slotting lithium can hydrolyze in water peels off into monolayer 1T phase MoS voluntarily2Nanometer sheet, then it is self-assembly of monolayer 1T phase molybdenum bisuphide/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 bisuphide/graphene composite material, be specifically related to one and prepare monolayer
The method of 1T phase molybdenum bisuphide/graphene composite material.
Background technology
Molybdenum bisuphide has typical sandwich layer structure, due to the Van der Waals force that its interlayer is relatively weak, it is also possible to stripping
From becoming the nanometer sheet of monolayer 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 monolayer 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 simulation2Peel off to monolayer from block, 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 power in cave improves (Phys.Rev.Lett.2010,105);Hinnemann et al. calculates nanometer by density letter formula
Level MoS2Expose activity edge absorption hydrogen Gibbs free energy, find that there is the strongest hydrogen adsorption ability at its edge, and have
Pt metal is equally close to the Hydrogen Evolution Performance of zero Gibbs free energy, thus infers the MoS of monolayer2Have and more expose 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, monolayer 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 are 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.Major part MoS in nature2Existing mutually with 2H, 1T with 3R phase belongs to metastable structure, under certain condition
2H phase can be changed into.MoS due to monolayer 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.Such as, 2H state MoS2Material
Material shows the characteristic of semiconductor that energy gap is 1.3-1.9eV, its by the number of plies number regulate the size of energy gap;
And the MoS of 1T state2Material then presents metallic character, and its superior electric conductivity is led at catalytic water decomposing hydrogen-production and super capacitor
Territory achieve important breakthrough (Advanced Energy Materials, 2016, DOI:10.1002/
Aenm.201502555).
Although monolayer MoS2Nano material is in the character of the aspect such as heat, electricity, light, mechanics and in field of optoelectronic devices
Potential application causes the extensive concern of scientific research personnel.But, general chemistry, Physical are difficult to prepare pure single layer structure
MoS2The monolayer molybdenum sulfide of nano material, especially different phase peels off preparation.Prepare monolayer MoS at present2Nano material main
Having micromechanical forces stripping method, chemical vapour deposition technique, lithium ion graft process and liquid chromatography ultrasound method etc., these stripping means are not only
Complex operation, complex process, and monolayer MoS2Yield extremely low, major part be thickness be few number of plies MoS of 1-100nm2Nanometer
Sheet, rather than monolayer MoS truly2.Monolayer MoS is prepared except being difficult to stripping expeditiously2Outside nanometer sheet, MoS2Nanometer
Sheet can only be peeled off and preserve in the such as high boiling organic solvent such as dimethylformamide and N-Methyl pyrrolidone, and these have
Machine solvent viscosity is big, boiling point is the highest, during centrifugal collection, and monolayer or few number of plies MoS2It is gathered into multilamellar MoS again2Receive
Rice sheet, thus limit monolayer MoS2Nanometer sheet is in some scientific researches or the exploration of industrial circle and application.
Lithium ion graft process is to peel off 1T phase MoS at present2Material most efficient method, Morrison et al. utilizes normal-butyl
Lithium is that lithium ion intercalator is embedded into MoS2Course of blocks is formed LixMoS2(x >=1) intercalation compound, then by with protic
Produced by solvent (usually water, it is also possible to select diluted acid) vigorous reaction, a large amount of hydrogen and heat are by MoS2Peel off, simultaneously
The MoS arrived2Induce distortion of lattice due to the insertion of lithium ion and form 1T phase (Mater.Res.Buu.1986,21,457).Should
Method is very sensitive to air and water due to butyl lithium reagent, has the biggest danger, and the process of slotting lithium is the veryest long, generally
Take several days weeks the most several, monolayer 1T phase MoS obtained2Yield is extremely low, to such an extent as to cannot carry out studying and answering in different field again
With.Zeng etc. insert lithium method by electrochemistry, and lithium ion is inserted into MoS2In block materials intercalation, make its shape by controlling voltage
Become LixMS2Phase, then carry out with water peeling off (Angew.Chem.InEd.2012,51,9052), although this method greatly reduces
The danger of operation and the waste of organic solvent, but electrode production process is complicated, MoS2Material conductivity is poor, is difficult to control
Ensure size of current and discharge time and insert lithium completely, cause charge stripping efficiency low.Additionally, MoS2Nanometer sheet is in real application research mistake
Cheng Zhong, often compound, to increase its electric conductivity with the material with carbon element such as agraphitic carbon, CNT, carbon fiber and Graphene.
Summary of the invention
Present invention solves the technical problem that the preparation that there is provided a kind of simple, safe efficient and applicable large-scale production
The method of monolayer 1T 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 1T phase at a certain temperature2MoS2Block, inserts lithium Li2MoS2Block hydrolyzes certainly in deionized water
Row is peeled off, then is self-assembled into monolayer 1T phase molybdenum bisuphide/graphene composite material, prepared monolayer with the graphene oxide added
1T phase molybdenum bisuphide/graphene composite material both can improve the electric conductivity of material, can effectively suppress again monolayer 1T phase two
The reunion of molybdenum sulfide.
The present invention adopts the following technical scheme that for solving above-mentioned technical problem, and one prepares monolayer 1T phase molybdenum bisuphide/stone
The method of ink alkene composite, it is characterised in that concretely comprise the following steps:
(1) ammonium thiomolybdate and lithium salt compound being pressed 1:2 mixed in molar ratio grind, the mixture after grinding is protected at noble gas
Protect down and be incubated 1-10h in 800-1200 DEG C, be cooled to room temperature and obtain inserting the 1T phase molybdenum sulfide block of lithium;
(2) being placed directly within deionized water by the 1T phase molybdenum sulfide block of slotting lithium, 5-30min is peeled off in assisting ultrasonic hydrolysis, then will
The suspension obtained is placed in a centrifuge, and obtains monolayer 1T phase MoS after being performing centrifugal separation on removing unstripped precipitate2Nanometer sheet
Suspension;
(3) monolayer 1T phase MoS is added graphene oxide into2In nanometer sheet suspension, ultrasonic disperse 5-10min, it is subsequently adding
Hydrazine hydrate continues ultrasonic 0.5-2h and obtains monolayer 1T phase MoS2/ graphene suspension;
(4) monolayer 1T phase MoS that will obtain2/ graphene suspension is removed with water and ethanol centrifuge washing on centrifuge respectively
Soluble impurity, is finally scattered in small molecule solvent preservation by precipitate monolayer 1T phase molybdenum bisuphide/graphene composite material,
Wherein monolayer 1T phase MoS2The thickness of nanometer sheet is less than 1nm.
Limit further, the lithium salt compound described in step (1) be Lithium hydrate, lithium chloride, lithium acetate, lithium carbonate,
One or more in lithium sulfate or lithium nitrate.
Limiting 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 monolayer 1T 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, methanol, ethanol, isopropanol, butanol, acetone,
N-Methyl pyrrolidone or N-METHYLFORMAMIDE.
The present invention compared with prior art has the advantage that
1, the present invention is with ammonium thiomolybdate and lithium salt compound as raw material, controls to synthesize slotting lithium by simple temperature
1T phase molybdenum sulfide block, the 1T phase molybdenum sulfide block of slotting lithium can hydrolyze in water peels off into monolayer 1T phase MoS voluntarily2Nanometer
Sheet, then it is self-assembly of monolayer 1T phase molybdenum bisuphide/graphene composite material with graphene oxide, and can be at water, ethanol
Deng stable existence in small molecule solvent;
2, monolayer 1T phase 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;
3, the present invention synthesis monolayer 1T phase molybdenum bisuphide/graphene composite material may be used for monolayer molybdenum sulfide light liberation of hydrogen,
The research in the field such as electro-catalysis and energy storage;
4, present invention process is simple to operate, and reaction condition is gentle, and agents useful for same is cheap, environmental protection.
Detailed description of the invention
By the following examples the foregoing of the present invention is described in further details, but this should be interpreted as this
The scope inventing above-mentioned theme is only limitted to below example, and all technology realized based on foregoing of the present invention belong to this
Bright scope.
Embodiment 1
Weigh the Lithium hydrate 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 shield, temperature programming to 800 DEG C, insulation
10h, then proceedes to logical argon and is naturally cooling to room temperature, obtain inserting the 1T phase molybdenum sulfide (Li of lithium2MoS4) block;Sulfur by slotting lithium
Changing molybdenum block to be placed in the container filling 100mL deionized water, ultrasonic disperse 10min, the suspension after dispersion at 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, adding 0.5mL mass fraction after ultrasonic disperse 10min is the hydrazine hydrate of 80%, continues super
Sound 0.5h obtains monolayer 1T phase MoS2/ graphene suspension;Monolayer 1T phase MoS that will obtain2/ graphene suspension at rotating speed is
Soluble impurity is removed, finally by precipitate monolayer 1T 3 times with water and ethanol centrifuge washing respectively on the centrifuge of 4000r/min
Phase molybdenum bisuphide/graphene composite material is scattered in 200mL deionized water preservation.The monolayer 1T phase molybdenum bisuphide/stone of gained
In ink 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 shield, temperature programming to 1200 DEG C, insulation
2h, then proceedes to logical argon and is naturally cooling to room temperature, obtain inserting the 1T phase molybdenum sulfide (Li of lithium2MoS4) block;Sulfuration by slotting lithium
Molybdenum block is placed in the container filling 200mL deionized water, ultrasonic disperse 10min, and the suspension after dispersion at 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, adding 1mL mass fraction after ultrasonic disperse 10min is the hydrazine hydrate of 80%, continues ultrasonic
0.5h obtains monolayer 1T phase MoS2/ graphene suspension;Monolayer 1T phase MoS that will obtain2/ graphene suspension at rotating speed is
Soluble impurity is removed, finally by precipitate monolayer 3 times with water and ethanol centrifuge washing respectively on the centrifuge of 10000r/min
1T phase molybdenum bisuphide/graphene composite material is scattered in 200mL dehydrated alcohol preservation.The monolayer 1T 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 shield, temperature programming to 1000 DEG C, insulation
5h, then proceedes to logical argon and is naturally cooling to room temperature, obtain inserting the 1T 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/ at rotating speed
Centrifugation precipitation on the centrifuge of min;Molybdenum disulfide content according to removing in precipitation rear suspension liquid adds 1:0.10 mass
The graphene oxide of ratio, adding 5mL mass fraction after ultrasonic disperse 10min is the hydrazine hydrate of 80%, continues ultrasonic 1h and obtains monolayer
1T phase MoS2/ graphene suspension;Monolayer 1T phase MoS that will obtain2/ graphene suspension rotating speed be 15000r/min from
Soluble impurity is removed, finally by precipitate monolayer 1T phase molybdenum bisuphide/stone 3 times with water and ethanol centrifuge washing respectively in scheming
Ink alkene composite is scattered in 200mL isopropanol preservation.Stone in the monolayer 1T phase molybdenum bisuphide/graphene composite material of gained
The content of ink 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
Being placed in corundum crucible by mixture after mill, is placed in tube furnace, logical argon shield, temperature programming to 900 DEG C, insulation
5h, then proceedes to logical argon and is naturally cooling to room temperature, obtain inserting the 1T 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 at rotating speed is
Centrifugation precipitation on the centrifuge of 1000r/min;Molybdenum disulfide content according to removing in precipitation rear suspension liquid adds 1:0.2
The graphene oxide of mass ratio, adding 10mL mass fraction after ultrasonic disperse 10min is the hydrazine hydrate of 80%, continues ultrasonic 2h and obtains
To monolayer 1T phase MoS2/ graphene suspension;Monolayer 1T phase MoS that will obtain2/ graphene suspension is 20000r/ at rotating speed
Soluble impurity is removed, finally by precipitate monolayer 1T phase two sulfur 3 times with water and ethanol centrifuge washing respectively on the centrifuge of min
Change molybdenum/graphene composite material and be scattered in 200mL N-Methyl pyrrolidone preservation.The monolayer 1T phase molybdenum bisuphide/stone of gained
In ink alkene composite, the content of Graphene is about 10%.
Embodiment above describes the ultimate principle of the present invention, principal character and advantage, the technical staff of the industry should
Understanding, the present invention is not restricted to the described embodiments, and the simply explanation present invention's described in above-described embodiment and description 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. the method preparing monolayer 1T phase molybdenum bisuphide/graphene composite material, it is characterised in that concretely comprise the following steps:
(1) ammonium thiomolybdate and lithium salt compound being pressed 1:2 mixed in molar ratio grind, the mixture after grinding is protected at noble gas
Protect down and be incubated 1-10h in 800-1200 DEG C, be cooled to room temperature and obtain inserting the 1T phase molybdenum sulfide block of lithium;
(2) being placed directly within deionized water by the 1T phase molybdenum sulfide block of slotting lithium, 5-30min is peeled off in assisting ultrasonic hydrolysis, then will
The suspension obtained is placed in a centrifuge, and obtains monolayer 1T phase MoS after being performing centrifugal separation on removing unstripped precipitate2Nanometer sheet
Suspension;
(3) monolayer 1T phase MoS is added graphene oxide into2In nanometer sheet suspension, ultrasonic disperse 5-10min, it is subsequently adding water
Close the hydrazine ultrasonic 0.5-2h of continuation and obtain monolayer 1T phase MoS2/ graphene suspension;
(4) monolayer 1T phase MoS that will obtain2/ graphene suspension is removed with water and ethanol centrifuge washing on centrifuge respectively can
Solubility impurity, is finally scattered in small molecule solvent preservation by precipitate monolayer 1T phase molybdenum bisuphide/graphene composite material, its
Middle monolayer 1T phase MoS2The thickness of nanometer sheet is less than 1nm.
The method preparing monolayer 1T phase molybdenum bisuphide/graphene composite material the most according to claim 1, its feature exists
In: the lithium salt compound described in step (1) is in Lithium hydrate, lithium chloride, lithium acetate, lithium carbonate, lithium sulfate or lithium nitrate
One or more.
The method preparing monolayer 1T phase molybdenum bisuphide/graphene composite material the most 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。
The method preparing monolayer 1T phase molybdenum bisuphide/graphene composite material the most according to claim 1, its feature exists
In: the graphene oxide described in step (3) and monolayer 1T phase MoS2MoS in nanometer sheet suspension2Mass ratio be 0.005-
0.2:1。
The method preparing monolayer 1T phase molybdenum bisuphide/graphene composite material the most according to claim 1, its feature exists
In: the small molecule solvent described in step (4) be water, methanol, ethanol, isopropanol, butanol, acetone, N-Methyl pyrrolidone or
N-METHYLFORMAMIDE.
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CN108682565A (en) * | 2018-06-12 | 2018-10-19 | 上海应用技术大学 | A kind of layer-layer graphene/molybdenum disulfide combination electrode material and preparation method thereof |
CN110911177A (en) * | 2019-12-04 | 2020-03-24 | 苏州大学 | Preparation method of asymmetric molybdenum disulfide/graphene micro supercapacitor |
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