CN103771517B - Method for preparing liquid phase dispersion-based two-dimensional MoS2 nanosheets - Google Patents

Method for preparing liquid phase dispersion-based two-dimensional MoS2 nanosheets Download PDF

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CN103771517B
CN103771517B CN201410022747.7A CN201410022747A CN103771517B CN 103771517 B CN103771517 B CN 103771517B CN 201410022747 A CN201410022747 A CN 201410022747A CN 103771517 B CN103771517 B CN 103771517B
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mos
nanometer sheet
preparation
mos2
dimentional
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CN103771517A (en
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王荣国
何亚飞
郝立峰
陆小龙
刘文博
矫维成
杨帆
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Harbin Institute of Technology
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Harbin Institute of Technology
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Abstract

The invention discloses a method for preparing liquid phase dispersion-based two-dimensional MoS2 nanosheets and relates to a method for preparing two-dimensional MoS2 nanosheets. The problems that the existing process for preparing the MoS2 nanosheets is complex, the thickness of the obtained MoS2 nanosheets are not close enough to a single layer and the concentration of the MoS2 nanosheets in suspension is low are solved. The preparation method comprises the following steps: 1, mixing MoS2 block powder with a dispersing solvent, thereby obtaining initial mixed liquor; 2, shearing the initial mixed liquor at a high speed; 3, performing ultrasonic treatment on the mixed liquor; 4, finally performing centrifugal treatment on the mixed liquor, standing, taking the supernatant, and obtaining the two-dimensional MoS2 nanosheet suspension. The process is simple and feasible, the fluorescence phenomenon of the obtained MoS2 nanosheet suspension is obviously enhanced, the thickness of the MoS2 nanosheets is closer to the single layer, and the concentration of the nanosheets is higher. The method is mainly applied to the fields of semiconductors, optoelectronic devices, aerospace, nondestructive testing and composite materials.

Description

A kind of two-dimentional MoS based on solution dispersion 2the preparation method of nanometer sheet
Technical field
The present invention relates to a kind of two-dimentional MoS 2the preparation method of nanometer sheet.
Background technology
Two-dimensional nano sheet (2D-nanasheets) is the thinnest a kind of function nano material, it have atom or molecule thickness and compared with thickness infinitely-great planar dimension.MoS 2be a kind of S-Mo-S stacking,vertical structure in layer, interlayer combines with faint Van der Waals force.Just because of this special structure, make to destroy MoS 2interlaminar action, prepare the MoS of individual layer 2nanometer sheet becomes possibility.The MoS of individual layer 2thickness is about block MoS 2the indirect band-gap semiconductor of to be band gap width be 1.2eV, its fluorescence (PL) signal is very weak.But the MoS of individual layer 2be direct band-gap semicondictor, its energy gap is 1.9eV, has very strong PL signal.The change of this character makes MoS 2nanometer sheet can produce some special reactions to electricity, magnetic, light etc.Theoretical and Experimental report shows MoS simultaneously 2band gap width with STRESS VARIATION, namely PL peak can with STRESS VARIATION.This makes it have huge application prospect at semiconductor applications.In addition, MoS 2" dangling bonds " and the thermostability of its excellence and mechanical property all make that there is application potential more widely.MoS 2nanometer sheet is described as " Graphene " of semiconductor applications, it by opto-electronic device and strongthener multi-functional in will show very large application prospect.
At present, individual layer MoS is obtained 2the method of nanometer sheet mainly contains micromechanics method, ion insertion method, reactive deposition method, solvent-thermal method etc.Micromechanics method prepares MoS by mechanically peel 2nanometer sheet, the MoS that this legal system is standby 2nanometer sheet comparatively small amt, can not widespread use actual production.The complicated process of preparation of ion insertion method is high to preparation environmental requirement.The MoS that reactive deposition legal system is standby 2nanometer sheet is second-rate.Solvent-thermal method is at preparation MoS 2nanometer sheet complex process, needs to add tensio-active agent, easily introduces impurity.Ultrasonic dispersion is the MoS of preparation preferably at present 2the method of nanometer sheet suspension, this method technical process is simple and easy to do, MoS 2nanometer sheet suspension also has more practical use.But prepare MoS by ultrasonic dispersion 2the concentration of nanometer sheet suspension is less, MoS 2the thickness low LCL of nanometer sheet is close to individual layer.In addition, the preparation technology of ultrasonic dispersion neither be very perfect in unification, needs constantly to carry out improving and optimize.
Summary of the invention
The present invention seeks to solve existing preparation MoS 2the complex process of nanometer sheet, the nanometer sheet thickness low LCL obtained is close to individual layer and MoS 2moS in nanometer sheet suspension 2the problem that nanometer sheet concentration is less, and a kind of two-dimentional MoS based on solution dispersion is provided 2the preparation method of nanometer sheet.
The present invention is based on the two-dimentional MoS of solution dispersion 2the preparation method of nanometer sheet follows these steps to realize:
One, by the MoS of natural hexagonal structure 2bulk powder mixes with dispersion solvent, preparation MoS 2initial mixing liquid;
Two, adopt high speed shear emulsification instrument to carry out high speed shear 20min ~ 100min with the initial mixing liquid of the shearing rate of 10000rpm ~ 20000rpm to step one, obtain the mixed solution after shearing treatment;
Three, the mixed solution after the shearing treatment obtained step 2 carries out supersound process, obtains the mixed solution after supersound process;
Four, the mixed solution after the supersound process obtained step 3 with the rotating speed of 1500rpm ~ 6000rpm carries out centrifugal treating, centrifugal complete after get supernatant liquid, leave standstill 22 ~ 26h, and then get the supernatant liquid of the reaction solution left standstill, obtain two-dimentional MoS 2nanometer sheet suspension;
Dispersion solvent wherein described in step one is 1-Methyl-2-Pyrrolidone (NMP), l-vinyl-2-pyrrolidone (NVP), dimethyl sulfoxide (DMSO) (DMSO) or dimethyl formamide (DMF).
The present invention is based on the two-dimentional MoS of solution dispersion 2the preparation method of nanometer sheet mainly comprises following advantage:
1, the present invention prepares two-dimentional MoS 2the technological operation of nanometer sheet suspension is simple, and equipment used is this area conventional instrument, and process cycle is short, lower to the requirement of process environments, with low cost.
2, the MoS of preparation 2the concentration of nanometer sheet suspension is comparatively large, output is high, good stability.Contrast known MoS 2the fluorescence phenomenon of nanometer sheet suspension obviously strengthens, MoS 2nanometer sheet thickness is about about 2nm, and the number of plies is approximately 1 ~ 2 layer, MoS 2the thickness of nanometer sheet is closer to individual layer.
3, the MoS of preparation 2nanometer sheet suspension selects common solvent, easily produces the liquid of impurity, the two-dimentional MoS of preparation without the need to adding tensio-active agent or intercalator etc. 2the purity of nanometer sheet suspension is high, and quality is good.The present invention is mainly used in the fields such as semi-conductor, opto-electronic device, aerospace, nondestructive testing and matrix material.
Accompanying drawing explanation
Fig. 1 is MoS prepared by embodiment one 2moS in nanometer sheet suspension 2the afm image of nanometer sheet;
Fig. 2 in Fig. 1 cut the gauge figure of partial cross section;
Fig. 3 is MoS prepared by embodiment one 2the fluorescence spectrum figure of nanometer sheet suspension.
Embodiment
Embodiment one: present embodiment is based on the two-dimentional MoS of solution dispersion 2the preparation method of nanometer sheet follows these steps to implement:
One, by the MoS of natural hexagonal structure 2bulk powder mixes with dispersion solvent, preparation MoS 2initial mixing liquid;
Two, adopt high speed shear emulsification instrument to carry out high speed shear 20min ~ 100min with the initial mixing liquid of the shearing rate of 10000rpm ~ 20000rpm to step one, obtain the mixed solution after shearing treatment;
Three, the mixed solution after the shearing treatment obtained step 2 carries out supersound process, obtains the mixed solution after supersound process;
Four, the mixed solution after the supersound process obtained step 3 with the rotating speed of 1500rpm ~ 6000rpm carries out centrifugal treating, centrifugal complete after get supernatant liquid, leave standstill 22 ~ 26h, and then get the supernatant liquid of the reaction solution left standstill, obtain two-dimentional MoS 2nanometer sheet suspension;
Dispersion solvent wherein described in step one is 1-Methyl-2-Pyrrolidone (NMP), l-vinyl-2-pyrrolidone (NVP), dimethyl sulfoxide (DMSO) (DMSO) or dimethyl formamide (DMF).
The MoS of the natural hexagonal structure that present embodiment step one uses 2bulk powder is by commercially available.
Present embodiment is based on the two-dimentional MoS of solution dispersion 2the preparation method of nanometer sheet utilizes specific intensive polar solvent to destroy MoS 2interlaminar action, recycling high speed shear emulsification instrument is to the MoS at specific intensive polar solvent 2impose strong shearing force, further destroy MoS 2interlaminar action, finally utilize ultrasonication, will the MoS of interlaminar action be destroyed 2spread out, under liquid phase state, prepare two-dimentional MoS 2nanometer sheet.
Embodiment two: MoS in the initial mixing liquid that present embodiment and embodiment one obtain unlike step one 2the concentration of bulk powder is 25mg/mL ~ 125mg/mL.Other step and parameter identical with embodiment one.
Embodiment three: present embodiment and embodiment one or two adopt high speed shear emulsification instrument to carry out high speed shear 30min ~ 60min with the initial mixing liquid of the shearing rate of 10000rpm ~ 15000rpm to step one unlike step 2.Other step and parameter identical with embodiment one or two.
Embodiment four: one of present embodiment and embodiment one to three are adopt power to be the probe sonication 1h ~ 3h of 600W ~ 800W unlike the supersound process described in step 3.Other step and parameter identical with one of embodiment one to three.
Embodiment five: one of present embodiment and embodiment one to three are adopt power to be the water bath sonicator process 1h ~ 8h of 150W ~ 240W unlike the supersound process described in step 3.Other step and parameter identical with one of embodiment one to three.
Embodiment four and five, when carrying out supersound process, in order to prevent solvent moisture absorption, can cover with preservative film and holding on the container of solvent.
Embodiment six: the mixed solution after the supersound process that one of present embodiment and embodiment one to five obtain step 3 with the rotating speed of 1500rpm ~ 3000rpm unlike step 4 carries out centrifugal treating.Other step and parameter identical with one of embodiment one to five.
Embodiment one: the present embodiment is based on the two-dimentional MoS of solution dispersion 2the preparation method of nanometer sheet follows these steps to implement:
One, by the MoS of natural for 4g hexagonal structure 2bulk powder mixes with 40mL1-N-methyl-2-2-pyrrolidone N-(NMP), preparation MoS 2initial mixing liquid;
Two, adopt high speed shear emulsification instrument to carry out high speed shear 60min with the initial mixing liquid of the shearing rate of 10000rpm to step one, obtain the mixed solution after shearing treatment;
Three, the mixed solution after the shearing treatment obtained step 2 carries out probe sonication 1h with the power of 600W, obtains the mixed solution after supersound process;
Four, the mixed solution after the supersound process obtained step 3 with the rotating speed of 1500rpm carries out centrifugal treating, gets supernatant liquid after centrifugal 45min, leaves standstill 24h, and then gets the supernatant liquid of the reaction solution left standstill, obtain two-dimentional MoS 2nanometer sheet suspension.
MoS prepared by the present embodiment 2nanometer sheet suspension is orange-yellow transparent liquid, and nanometer sheet suspension, in a vacuum after solvent evaporated, is pale yellow powder.
Fig. 1 and Fig. 2 is MoS prepared by the present embodiment 2moS in nanometer sheet suspension 2the afm image of nanometer sheet and the gauge in cross section.As can be seen from the figure, MoS 2nanometer sheet thickness is about about 2nm, and the number of plies is approximately 1 ~ 2 layer.
Fig. 3 is the FP-6500 fluorescence spectrophotometer selecting Japanese JASCO company to produce, the fluorescence spectrum figure recorded when excitation wavelength is 514nm, and wherein 1 represents MoS prepared by the present embodiment 2nanometer sheet suspension, 2 represent the MoS not carrying out high speed shear process 2nanometer sheet suspension, 3 represent MoS 2bulk powder, 4 represent 1-Methyl-2-Pyrrolidone (NMP).As can be seen from the figure: compare the sample do not sheared, through the MoS of high speed shear dispersion preparation 2the fluorescent effect of nanometer sheet suspension is stronger, and intensity approximately improves 32%, and this shows the MoS prepared by the present invention 2the concentration of nanometer sheet suspension is larger, MoS 2the thickness of nanometer sheet is closer to individual layer.
Embodiment two: the present embodiment is based on the two-dimentional MoS of solution dispersion 2the preparation method of nanometer sheet follows these steps to implement:
One, by the MoS of natural for 4g hexagonal structure 2bulk powder mixes with 40ml1-N-methyl-2-2-pyrrolidone N-(NMP), preparation MoS 2initial mixing liquid;
Two, adopt high speed shear emulsification instrument to carry out high speed shear 30min with the initial mixing liquid of the shearing rate of 10000rpm to step one, obtain the mixed solution after shearing treatment;
Three, the mixed solution after the shearing treatment obtained step 2 carries out water bath sonicator process 1h with the power of 240W, obtains the mixed solution after supersound process;
Four, the mixed solution after the supersound process obtained step 3 with the rotating speed of 1500rpm carries out centrifugal treating, gets supernatant liquid after centrifugal 45min, leaves standstill 24h, and then gets the supernatant liquid of the reaction solution left standstill, obtain two-dimentional MoS 2nanometer sheet suspension.
Two-dimentional MoS prepared by the present embodiment 2nanometer sheet suspension records its relative maximum fluorescence intensity when excitation wavelength is 514nm be 703, and the relative maximum fluorescence intensity comparing the sample do not sheared is 597, and fluorescence intensity approximately improves 18%.

Claims (6)

1. the two-dimentional MoS based on solution dispersion 2the preparation method of nanometer sheet, is characterized in that the two-dimentional MoS based on solution dispersion 2the preparation method of nanometer sheet follows these steps to realize:
One, by the MoS of natural hexagonal structure 2bulk powder mixes with dispersion solvent, preparation MoS 2initial mixing liquid;
Two, adopt high speed shear emulsification instrument to carry out high speed shear 20min ~ 100min with the initial mixing liquid of the shearing rate of 10000rpm ~ 20000rpm to step one, obtain the mixed solution after shearing treatment;
Three, the mixed solution after the shearing treatment obtained step 2 carries out supersound process, obtains the mixed solution after supersound process;
Four, the mixed solution after the supersound process obtained step 3 with the rotating speed of 1500rpm ~ 6000rpm carries out centrifugal treating, centrifugal complete after get supernatant liquid, leave standstill 22 ~ 26h, and then get the supernatant liquid of the reaction solution left standstill, obtain two-dimentional MoS 2nanometer sheet suspension;
Dispersion solvent wherein described in step one is 1-Methyl-2-Pyrrolidone, l-vinyl-2-pyrrolidone, dimethyl sulfoxide (DMSO) or dimethyl formamide.
2. a kind of two-dimentional MoS based on solution dispersion according to claim 1 2the preparation method of nanometer sheet, is characterized in that MoS in the initial mixing liquid that step one obtains 2the concentration of bulk powder is 25mg/mL ~ 125mg/mL.
3. a kind of two-dimentional MoS based on solution dispersion according to claim 1 2the preparation method of nanometer sheet, is characterized in that step 2 adopts high speed shear emulsification instrument to carry out high speed shear 30min ~ 60min with the initial mixing liquid of the shearing rate of 10000rpm ~ 15000rpm to step one.
4. a kind of two-dimentional MoS based on solution dispersion according to claim 1 2the preparation method of nanometer sheet, the supersound process that it is characterized in that described in step 3 adopts power to be the probe sonication 1h ~ 3h of 600W ~ 800W.
5. a kind of two-dimentional MoS based on solution dispersion according to claim 1 2the preparation method of nanometer sheet, the supersound process that it is characterized in that described in step 3 adopts power to be the water bath sonicator process 1h ~ 8h of 150W ~ 240W.
6. a kind of two-dimentional MoS based on solution dispersion according to claim 1 2the preparation method of nanometer sheet, is characterized in that the mixed solution after the supersound process that step 4 obtains step 3 with the rotating speed of 1500rpm ~ 3000rpm carries out centrifugal treating.
CN201410022747.7A 2014-01-17 2014-01-17 Method for preparing liquid phase dispersion-based two-dimensional MoS2 nanosheets Expired - Fee Related CN103771517B (en)

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