CN107384390A - A kind of preparation method of molybdenum disulfide quantum dot - Google Patents
A kind of preparation method of molybdenum disulfide quantum dot Download PDFInfo
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- CN107384390A CN107384390A CN201710633894.1A CN201710633894A CN107384390A CN 107384390 A CN107384390 A CN 107384390A CN 201710633894 A CN201710633894 A CN 201710633894A CN 107384390 A CN107384390 A CN 107384390A
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- molybdenum disulfide
- quantum dot
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
- C09K11/08—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials
- C09K11/67—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing refractory metals
- C09K11/68—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing refractory metals containing chromium, molybdenum or tungsten
- C09K11/681—Chalcogenides
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y20/00—Nanooptics, e.g. quantum optics or photonic crystals
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
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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
Abstract
The present invention relates to a kind of preparation method of molybdenum disulfide quantum dot, comprise the following steps：(1) molybdenum disulfide powder of the 150 250m g particle diameters no more than 4 μm is placed in mortar, adds 0.5 1.0g ionic liquids and ground in mortar, obtain the first dispersion liquid；(2) first the first dispersion liquid of organic solvent diluting is used, precipitation is collected by centrifugation；(3) described precipitation is redissolved in the second organic solvent and is transferred to closed glass container, be placed in supersonic wave cleaning machine and handled under the conditions of water bath with thermostatic control, stood after gained reaction solution is cooled into room temperature, collected 90% supernatant liquor, obtain the second dispersion liquid；(4) added in glass container, shaken up using the second organic solvent, repeat step described in (3)；(5) second dispersion liquid is evaporated, and be redissolved in deionized water, obtain molybdenum disulfide quantum dot solution.The preparation method of the present invention can obtain that monodispersity is good, microminiature molybdenum disulfide quantum dot of size uniform, easily realize inexpensive industrialization production.
Description
Technical field
The present invention relates to novel nano-material field, more particularly to a kind of preparation method of molybdenum disulfide quantum dot.
Background technology
As the two-dimension nano materials of a species graphene, platelike molybdenumdisulfide nano material has many unique physics
Chemical characteristic.The band gap of molybdenum disulfide nano material is relevant with the number of plies, and when peeling off to individual layer, its semiconductor gap is from indirect belt
Gap structure is converted into direct band gap result, causes photon absorption cross sections also bigger than graphene and noble metal nano particles, its
Fluorescence quantum efficiency is also greatly enhanced.Specific surface area is big, photoabsorption cross-section is big, quantum efficiency is high, good mechanical property, band gap
Unique structure makes molybdenum disulfide nano material have in fields such as photoelectric device, sensor, catalysis, battery, storage and biomedicines
Have broad application prospects.And molybdenum disulfide quantum dot its there is extra small size, thus with bigger specific surface area, stronger
Quantum confinement and boundary effect, sensor, optical probe and treatment of cancer etc. have more application prospect, therefore, two sulphur
That changes molybdenum quantum dot prepares great realistic meaning.
At present, preparing the method for molybdenum disulfide quantum dot includes mechanical stripping method (such as polishing), chemical synthesis, chemistry
Meteorological lamination, laser ablation, electron beam etching method etc..Mechanical stripping method prepares quantum dot low yield, time-consuming；Chemical synthesis
Quantum dot surface prepared by method usually contains part, is unfavorable for electric transmission；Chemical vapor lamination, laser ablation, electron beam are carved
Etching method can not on a large scale and high efficiency prepares quantum dot.Application publication number CN105271411A, denomination of invention:A kind of curing
The preparation method of molybdenum quantum dot, comprises the following steps：(1) molybdenum disulfide powder is dispersed in absolute ethyl alcohol；Into the solution
Sodium hydroxide, addition amount of sodium hydroxide 0.5-3mg/mL are added, ultrasound obtains mixed solution after mixing；(2) by step (1) institute
State mixed solution to be transferred in reactor, seal, react 3-24h in 100-200 DEG C of baking oven, naturally cool to room temperature, filter
Gained filtrate is collected afterwards；(3) filtrate obtained by step (2) is dialysed to neutrality in bag filter, goes removal of impurity small molecule, after drying
Molybdenum disulfide quantum dot is obtained, the molybdenum disulfide quantum dot is with the difference of excitation wavelength, the hair of molybdenum disulfide quantum dot
It is also different to penetrate optical wavelength, wherein maximum excitation wavelength is 370nm, and maximum emission wavelength now is 461nm, belongs to visible
Optical range.This is simple to operate, green, and cost is low, and process conditions are easily achieved, and prepared molybdenum disulfide quantum dot has
Excellent dispersiveness, water solubility and strong fluorescence.In the side such as opto-electronic device, lithium ion battery, bio-imaging, photoelectrocatalysis
Face has potential application value.But sodium hydroxide is needed to be used as a kind of burn into intercalation simultaneously, peel off in course of reaction
Reagent, while large scale molybdenum disulfide surface is corroded, insert it between layers, obtain small size molybdenum disulfide quantum
Point.But sodium hydroxide environmental pollution is bigger, and need to react using polytetrafluoroethyllining lining reactor, be unfavorable for big
Large-scale production, and production requirement is high.Therefore a kind of high yield, the preparation method of prepare with scale molybdenum disulfide quantum dot are developed
It is extremely urgent.
The content of the invention
The invention provides a kind of preparation method of molybdenum disulfide quantum dot, solves existing molybdenum disulfide quantum dot preparation side
Method low yield, time-consuming, can not be on a large scale and the problem of high efficiency prepares quantum dot.
In order to solve the above technical problems, the technical solution adopted by the present invention is：
A kind of preparation method of molybdenum disulfide quantum dot, comprises the following steps：
(1) molybdenum disulfide powder of the 150-250m g particle diameters no more than 4 μm is placed in mortar, adds 0.5-1.0g ions
Liquid is simultaneously ground in mortar, obtains the first dispersion liquid；
(2) first the first dispersion liquid of organic solvent diluting is used, precipitation is collected by centrifugation；
(3) described precipitation is redissolved in the second organic solvent and is transferred to closed glass container, it is clear to be placed in ultrasonic wave
Handle under the conditions of water bath with thermostatic control in washing machine, stood after gained reaction solution is cooled into room temperature, collect 90% supernatant liquor, obtain the
Two dispersion liquids；
(4) added in glass container, shaken up using the second organic solvent, repeat step described in (3)；
(5) second dispersion liquid is evaporated, and be redissolved in deionized water, it is molten to obtain molybdenum disulfide quantum dot
Liquid.
Preferably：In step (1), described mortar is agate mortar, and the milling time is 0.5-1 hours.
Preferably：In step (2), described supersound process is：Ultrasonic power is 100-150W, ultrasonic time 3.5-
4.5 hours, the water bath with thermostatic control temperature was 85-95 DEG C.
Preferably：The ionic liquid is 1- butyl -3- methylimidazole hexafluorophosphates.
Preferably：First organic solvent is acetone；Second organic solvent is 1-METHYLPYRROLIDONE, N, N- bis-
NMF, dimethyl sulfoxide, the one or more of methylimidazole quinoline and ethanol.
Preferably：The particle diameter of described molybdenum disulfide powder is less than 2 μm.
Preferably：The centrifugal rotational speed is 8000-12000 revs/min, and centrifugation time is 10-20 minutes.
Preferably：The concentration of molybdenum disulfide quantum dot is 2g/L in the solution of the step (5).
Preferably：Second dispersion liquid is evaporated in baking oven under vacuum, and the temperature is 80-120 DEG C.
Preferably：In step (3), described closed glass container is 50mL serum bottles or other similar vessels.
Present invention provides a kind of molybdenum disulfide quantum dot, the size of the molybdenum disulfide quantum dot is 1-1.5nm.
Beneficial effect of the present invention：
The preparation method of the molybdenum disulfide quantum dot of the present invention, realizes the stripping and fragmentation to molybdenum disulfide block, this
Method technique is simple, it is time-consuming it is short, yield is high, favorable repeatability, be adapted to large-scale production, compared to current mechanical stripping method and change
The methods of learning meteorological lamination has obvious advantage, can obtain that monodispersity is good, microminiature molybdenum disulfide quantum of size uniform
Point, easily realize inexpensive industrialization production.
The preparation method of molybdenum disulfide quantum dot realizes prepared by the extensive industrialization from molybdenum disulfide block to quantum dot,
Base is established for application of the molybdenum disulfide quantum dot in fields such as photoelectric device, sensor, catalysis, battery, storage and biomedicines
Plinth.
The molybdenum disulfide quantum dot that the preparation method of the present invention is prepared, the size of the molybdenum disulfide quantum dot is in 1-
1.5nm, particle diameter distribution is narrower, and size is smaller, shows obvious absorption characteristic in ultraviolet light visual field, can apply to prepare
The biomedical frontier fields such as photo-thermal therapy medicine, optical bio label, sensor.
Intermediate ion liquid of the present invention is added in mortar and molybdenum disulfide powder is ground together, the surface energy of this ionic liquid
Very close with the surface energy of molybdenum disulfide, therefore, this ionic liquid can effectively weaken interlayer Van der Waals force, efficiently will
Molybdenum disulfide is peeled off into few layer of nanometer sheet.In addition, ionic liquid is the green organic solvent that can be recycled, environment will not be caused
Pollution.
In the step (3) of the present invention, the energy of ultrasound offer, which can weaken interlayer Van der Waals force, makes it further peel off simultaneously
A small amount of quantum dot is obtained, the energy that high temperature provides can make molybdenum disulfide nano sheet be isolated into small size so as to gradually form quantum
Point, both act synergistically so that the yield of molybdenum disulfide quantum dot greatly improves.
Brief description of the drawings
In order to illustrate more clearly about the embodiment of the present invention or technical scheme of the prior art, below will be to embodiment or existing
There is the required accompanying drawing used in technology description to be briefly described, it should be apparent that, drawings in the following description are only this
Some embodiments of invention, for those of ordinary skill in the art, on the premise of not paying creative work, can be with
Other accompanying drawings are obtained according to these accompanying drawings.
Fig. 1 is the ultraviolet-visible absorption spectroscopy of molybdenum disulfide quantum dot in deionized water made from the embodiment of the present invention 1；
Fig. 2 is the low power transmission electron microscope image of molybdenum disulfide quantum dot made from the embodiment of the present invention 1
(TEM)；
Fig. 3 is the high power transmission electron microscope image of molybdenum disulfide quantum dot made from the embodiment of the present invention 1
(HRTEM)；
Fig. 4 is the AFM image (AFM) of molybdenum disulfide quantum dot made from the embodiment of the present invention 1.
Embodiment
Below in conjunction with the accompanying drawing in the embodiment of the present invention, the technical scheme in the embodiment of the present invention is carried out clear, complete
Site preparation describes, it is clear that described embodiment is only part of the embodiment of the present invention, rather than whole embodiments.It is based on
Embodiment in the present invention, those of ordinary skill in the art are obtained every other under the premise of creative work is not made
Embodiment, belong to the scope of protection of the invention.
Embodiment 1
A kind of preparation method of molybdenum disulfide quantum dot, comprises the following steps：
(1) molybdenum disulfide powder of the 200mg particle diameters less than 2 μm is placed in agate mortar, adds 0.5g1- butyl -3- first
Base limidazolium hexafluorophosphate is simultaneously ground 0.5 hour in agate mortar, obtains the first dispersion liquid；
(2) the first dispersion liquid is diluted using 10mL acetone, centrifuged 15 minutes under 10000 revs/min, collect precipitation；
(3) described precipitation is redissolved in 30mLN- methyl pyrrolidones and is transferred to closed glass container, be placed in super
Handled 4 hours, ultrasonic power 120W under the conditions of water bath with thermostatic control in sound wave cleaning machine, water bath with thermostatic control temperature is 90 DEG C；By gained
Reaction solution stands 2 hours after being cooled to room temperature, collects 90% supernatant liquor, obtains the second dispersion liquid；
(4) added in glass container, shaken up using 27mLN- methyl pyrrolidones, repeat step described in (3)；
(5) second dispersion liquid is evaporated down in an oven, and be redissolved in deionized water, molybdenum disulfide in solution
The concentration of quantum dot is 2g/L, obtains molybdenum disulfide quantum dot solution.
The molybdenum disulfide quantum dot of the gained of the present embodiment 1 is relatively stable, can deposit at room temperature 6 months.By the present embodiment 1
The molybdenum disulfide quantum dot of gained is characterized, as a result as shown in 1-4 figures.Fig. 1 can be seen that molybdenum disulfide quantum dot in 250-
600nm regions show obvious absorption characteristic, and neat absorption peak is about in 270nm；It can be seen that obtained curing in Fig. 2
Molybdenum quantum dot monodispersity is good, size uniform, and its size is in 3nm or so；It can clearly be seen that molybdenum disulfide quantum dot is former in Fig. 3
The lattice fringe of sublayer, wherein, spacing of lattice 0.23nm, to (103) crystal face for molybdenum disulfide quantum dot；Can in Fig. 4
To find out obtained molybdenum disulfide quantum dot thickness as 1-2nm, corresponding to 1-3 layer molybdenum disulfide.
Embodiment 2
A kind of preparation method of molybdenum disulfide quantum dot, comprises the following steps：
(1) molybdenum disulfide powder of 2-4 μm of 150mg particle diameters is placed in agate mortar, adds 0.8g1- butyl -3- methyl
Limidazolium hexafluorophosphate is simultaneously ground 0.5 hour in agate mortar, obtains the first dispersion liquid；
(2) the first dispersion liquid is diluted using 10mL acetone, centrifuged 20 minutes under 8000 revs/min, collect precipitation；
(3) described precipitation is redissolved in 30mLN- methyl pyrrolidones and is transferred to closed glass container, be placed in super
Handled 4.5 hours, ultrasonic power 100W under the conditions of water bath with thermostatic control in sound wave cleaning machine, water bath with thermostatic control temperature is 85 DEG C；By institute
Obtain after reaction solution is cooled to room temperature and stand 2 hours, collect 90% supernatant liquor, obtain the second dispersion liquid；
(4) added in glass container, shaken up using 27mLN- methyl pyrrolidones, repeat step described in (3)；
(5) second dispersion liquid is evaporated down in an oven, and be redissolved in deionized water, molybdenum disulfide in solution
The concentration of quantum dot is 2g/L, obtains molybdenum disulfide quantum dot solution.
Molybdenum disulfide quantum dot obtained by the present embodiment is relatively stable, can deposit at room temperature 6 months.By the present embodiment institute
The molybdenum disulfide quantum dot obtained is characterized, as a result similar to Example 1.
Embodiment 3
A kind of preparation method of molybdenum disulfide quantum dot, comprises the following steps：
(1) molybdenum disulfide powder of the 250mg particle diameters less than 2 μm is placed in agate mortar, adds 1.0g1- butyl -3- first
Base limidazolium hexafluorophosphate is simultaneously ground 0.5 hour in agate mortar, obtains the first dispersion liquid；
(2) the first dispersion liquid is diluted using 10mL acetone, centrifuged 10 minutes under 12000 revs/min, collect precipitation；
(3) described precipitation is redissolved in 30mLN- methyl pyrrolidones and is transferred to closed glass container, be placed in super
Handled 3.5 hours, ultrasonic power 150W under the conditions of water bath with thermostatic control in sound wave cleaning machine, water bath with thermostatic control temperature is 95 DEG C；By institute
Obtain after reaction solution is cooled to room temperature and stand 2 hours, collect 90% supernatant liquor, obtain the second dispersion liquid；
(4) added in glass container, shaken up using 27mLN- methyl pyrrolidones, repeat step described in (3)；
(5) second dispersion liquid is evaporated down in an oven, and be redissolved in deionized water, molybdenum disulfide in solution
The concentration of quantum dot is 2g/L, obtains molybdenum disulfide quantum dot solution.
Molybdenum disulfide quantum dot obtained by the present embodiment is relatively stable, can deposit at room temperature 6 months.By the present embodiment 1
The molybdenum disulfide quantum dot obtained is characterized, as a result similar to Example 1.
The foregoing is merely illustrative of the preferred embodiments of the present invention, is not intended to limit the invention, all essences in the present invention
God any modification, equivalent substitution and improvements made etc., should be included in the scope of the protection with principle.
Claims (10)
1. a kind of preparation method of molybdenum disulfide quantum dot, it is characterised in that comprise the following steps：
(1) molybdenum disulfide powder of the 150-250mg particle diameters no more than 4 μm is placed in mortar, adds 0.5-1.0g ionic liquids
And ground in mortar, obtain the first dispersion liquid；
(2) first the first dispersion liquid of organic solvent diluting is used, precipitation is collected by centrifugation；
(3) described precipitation is redissolved in the second organic solvent and is transferred to closed glass container, be placed in supersonic wave cleaning machine
Handle under the conditions of middle water bath with thermostatic control, stood after gained reaction solution is cooled into room temperature, collect 90% supernatant liquor, obtain second point
Dispersion liquid；
(4) added in glass container, shaken up using the second organic solvent, repeat step described in (3)；
(5) second dispersion liquid is evaporated, and be redissolved in deionized water, obtain molybdenum disulfide quantum dot solution.
2. a kind of preparation method of molybdenum disulfide quantum dot as claimed in claim 1, it is characterised in that described in step (1)
Mortar be agate mortar, the milling time is 0.5-1 hours.
3. a kind of preparation method of molybdenum disulfide quantum dot as claimed in claim 1, it is characterised in that described in step (2)
Supersound process be：Ultrasonic power is 100-150W, and ultrasonic time is 3.5-4.5 hours, and the water bath with thermostatic control temperature is 85-95
℃。
4. a kind of preparation method of molybdenum disulfide quantum dot as claimed in claim 1, it is characterised in that the ionic liquid is
1- butyl -3- methylimidazole hexafluorophosphates.
5. a kind of preparation method of molybdenum disulfide quantum dot as claimed in claim 1, it is characterised in that described first is organic molten
Agent is acetone；Second organic solvent is 1-METHYLPYRROLIDONE, N,N-dimethylformamide, dimethyl sulfoxide, dimethyl miaow
The one or more of oxazoline and ethanol.
A kind of 6. preparation method of molybdenum disulfide quantum dot as claimed in claim 1, it is characterised in that described molybdenum disulfide
The particle diameter of powder is less than 2 μm.
7. a kind of preparation method of molybdenum disulfide quantum dot as claimed in claim 1, it is characterised in that the centrifugal rotational speed is
8000-12000 revs/min, centrifugation time is 10-20 minutes.
A kind of 8. preparation method of molybdenum disulfide quantum dot as claimed in claim 1, it is characterised in that the 3rd dispersion liquid
The concentration of middle molybdenum disulfide quantum dot is 2g/L.
A kind of 9. preparation method of molybdenum disulfide quantum dot as claimed in claim 1, it is characterised in that second dispersion liquid
It is evaporated under vacuum in baking oven, the temperature is 80-120 DEG C.
A kind of 10. molybdenum disulfide quantum dot, it is characterised in that：The size of described molybdenum disulfide quantum dot is 1-1.5nm.
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| CN110108697A (en) * | 2019-06-25 | 2019-08-09 | 北威(重庆)科技股份有限公司 | Surface enhanced Raman scattering micro-nano chip and preparation method thereof, application and Raman spectrum test macro |
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| CN110655110A (en) * | 2019-11-03 | 2020-01-07 | 台州学院 | Molybdenum disulfide with atomic layer step and preparation method thereof |
| CN112340710A (en) * | 2020-11-19 | 2021-02-09 | 太原理工大学 | Preparation method of high-quality tellurium quantum dots |
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| CN110108697A (en) * | 2019-06-25 | 2019-08-09 | 北威(重庆)科技股份有限公司 | Surface enhanced Raman scattering micro-nano chip and preparation method thereof, application and Raman spectrum test macro |
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| CN110655110B (en) * | 2019-11-03 | 2021-11-23 | 台州学院 | Molybdenum disulfide with atomic layer step and preparation method thereof |
| CN112340710A (en) * | 2020-11-19 | 2021-02-09 | 太原理工大学 | Preparation method of high-quality tellurium quantum dots |
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