CN108753291A - The preparation method of oil-soluble fluorescent TMDs quantum dots and its colloid - Google Patents
The preparation method of oil-soluble fluorescent TMDs quantum dots and its colloid Download PDFInfo
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Abstract
The present invention relates to technical field of nanometer material preparation, more particularly to the preparation method of a kind of oil-soluble fluorescent TMDs quantum dots and its colloid；Transition metal sulphur compound is added into cyclohexanone including (1), suspension is made；(2) suspension is carried out being heated to reflux processing, cooling and standings after reflux；(3) it takes the supernatant liquor after standing to carry out centrifugal treating, collects centrifuged supernatant later and carry out rotary distillation, obtain oil-soluble TMDs quantum dots.Advantageous effect of the present invention is：Method is simple, and mild condition safety, equipment cost is low, and preparation efficiency is high, is handled without later purification.
Description
Technical field
The present invention relates to technical field of nanometer material preparation, more particularly to a kind of oil-soluble fluorescent TMDs quantum dots and its glue
The preparation method of body.
Background technology
Quantum dot (Quantum Dots, QDs) is zero-dimension nano semi-conducting material, has a series of unique photoelectric properties,
It is widely used in fields such as solar cell, luminescent device, biomedicines.Two-dimentional Transition-metal dichalcogenide (TMDs) is
Refer to and X-M-X class sandwich structure chemical combination objects are formed by by transiting group metal elements (M) and sulfur family nonmetalloid (X), such as
MoS2、WS2Deng.People are concentrated mainly on micron and nanoscale to TMDs researchs all the time.As material technology develops, people
Find by further decreasing scantling, MoS2、WS2It can be mutated direct band gap material, physics, chemistry from indirect band gap
Property mutates, such as have compared with high-fluorescence quantum yield, extinction coefficient, it is anti-drift ability, wider excitation spectrum range and
Superior electron transfer rate etc..It can be applied to the fields such as fluorescent ink, photoelectric device, biomarker, fluorescence probe.
The basis material of fluorescent electronic material ink at present, based on II-VI group quantum dot, such as CdSe, CdSe/CdS
Deng wherein harmful heavy metals such as cadmium are unfavorable for environmental protection.In addition, launch wavelength is 400-500nm II-VI group quantum dots
Preparation it is also extremely difficult.And MoS2、WS2Quantum dot emission spectrum range is just Chong Die with this range.
Therefore, oil-soluble fluorescence MoS is prepared2、WS2Quantum dot is of great significance to preparing fluorescent electronic material ink.
Currently, oil-soluble fluorescent MoS2、WS2Quantum dot prepares the hot method of primary solvent, hot injection method etc., published at present
Scheme is as follows：
1) Hongtao et al. (Inorganic Chemistry, 2008,47, (5):1428-1433.) with hexacarbonylmolybdenum sulphur
Powder is precursor, uses tri octyl phosphine for ligand, and octadecylene is solvent, goes out the smaller MoS of size with solvent structure2Quantum
Point.
2) (Chemistry ofMaterials, 2011,23 (17) ClaudiaAltavilla et al.:3879-3885.),
Using (NH4)2MoS4For precursor, oleyl amine is solvent, obtains MoS at high temperature2And WS2Quantum dot.
3) Yueli Liu et al. people (Journal ofMaterials Science:Materials in Electronics,
2017,28(18):13633-13637) with molybdenum chloride and N, N ' rhenocure CAs are molybdenum source and sulphur source, and MoS is prepared with hot note method2
Quantum dot.
In the above embodiments, although oil-soluble TMDs quantum dots and its colloid can be obtained, quantum dot building-up process,
It is related to a large amount of toxic solvents, technological requirement is harsh, and if you need to high temperature, anhydrous and oxygen-free environment etc., selectable precursor type is also limited.
Product later purification process is complicated, and yield is relatively low.
Therefore it is badly in need of the fluorescence transition that a kind of simple, effective method of development prepares oil-soluble, high fluorescence quantum yield
Metal sulfide quantum dots.
Invention content
The technical problem to be solved in the present invention is that the preparation method of existing oil-soluble fluorescent TMDs quantum dots is complicated, uneasy
Entirely.
In order to solve the above technical problems, the technical solution used in the present invention is：A kind of oil-soluble fluorescent TMDs quantum dots
Preparation method, include the following steps：
(1) transition metal sulphur compound is added into cyclohexanone, suspension is made；
(2) suspension is carried out being heated to reflux processing, cooling and standings after reflux；
(3) it takes the supernatant liquor after standing to carry out centrifugal treating, collects the supernatant after centrifugation later and carry out rotary distillation,
Obtain oil-soluble TMDs quantum dots.
The solvent degree of nano material in a solvent can use Hansen Solubility Parameter theoretical (HSP) description.I.e. nano material with
The dispersion force of solvent, permanent dipole force, hydrogen bond difference are smaller, and solubility is bigger in a solvent.Specific formula：
Wherein, δD,sol、δP,sol、δH,solRespectively solvent dispersion force, permanent dipole force, hydrogen bond.δD,NS、δP,NS、δH,NSPoint
It Wei not nano particle dispersion force, permanent dipole force, hydrogen bond.RaIt is worth smaller, solubility is bigger in a solvent for nano material.MoS2Color
Dissipating power, permanent dipole force, hydrogen bond is respectively：17-19MPa0.5,6-12MPa0.5,4.5-8.4MPa0.5。WS2Dispersion force, permanent idol
Strongly, hydrogen bond is respectively：16-18MPa0.5,5-14MPa0.5,2-19MPa0.5。
In the above-mentioned technical solutions, selected solvent cyclohexanone dispersion force, permanent dipole force, hydrogen bond are respectively：
17.2MPa0.5,10.6MPa0.5,4.8MPa0.5, with MoS2, WS2Etc. corresponding parametric values it is very close.Therefore, MoS2、WS2Deng
There is higher solubility in cyclohexanone.Using cyclohexanone as solvent, the method by being simply heated to reflux removes MoS2、WS2Deng can be with
Obtain the MoS of higher yields2、WS2Quantum dot.
Further, transition metal sulphur compound is MoS in the step (1)2、WS2Deng.
Further, in the step (1) transition metal sulphur compound and cyclohexanone according to 10-400mg：10-100ml's
Mass volume ratio mixes.
Further, the step (1) is mixed using magnetic agitation mode, and incorporation time is 8-12 minutes.
Further, the heating temperature in the step (2) is 130-140 DEG C, and return time is 10-12 hours, is being returned
Magnetic agitation state is kept during stream.
Further, the centrifuge speeds in the step (3) are 12000r/min, centrifugation time 10min.
Further, the rotary distillation condition in the step (3) is as follows：Temperature be 120 DEG C, relative degree of vacuum be-
40KPa。
It is another object of the present invention to provide a kind of preparation methods of oil-soluble fluorescent TMDs quantum dot colloids, use
The oil-soluble TMDs quantum dots that the above method is prepared are scattered in nonpolar solvent, obtain oil-soluble fluorescent TMDs quantum dispensings
Body.
The nonpolar solvent includes but not limited to hexane, hexamethylene, benzene, toluene, dichloromethane, chloroform, carbonic acid diformazan
Ester or ethyl acetate.
The beneficial effects of the present invention are：Method is simple, and mild condition safety, equipment cost is low, and preparation efficiency is high, is not necessarily to
Later purification processing.
Description of the drawings
Fig. 1 is the transmission electron microscope picture of product prepared by the embodiment of the present invention 1；
Fig. 2 is the transmission electron microscope picture of product prepared by the embodiment of the present invention 5；
Fig. 3 is the absorption of product and fluorescent emission collection of illustrative plates prepared by the embodiment of the present invention 1；
Fig. 4 is the absorption of product and fluorescent emission collection of illustrative plates prepared by the embodiment of the present invention 5；
Fig. 5 is the X diffraction patterns of product prepared by the embodiment of the present invention 1；
Fig. 6 is the X diffraction patterns of product prepared by the embodiment of the present invention 5.
Specific implementation mode
The present invention is further illustrated by 1-8 with reference to embodiments, and in following embodiment, reagent and instrument come
Source is as follows：
One, reagent：
MoS2：Purchased from (Zhengzhou Kingsoft Chemical Co., Ltd., 44 μm, 99.9%)；
WS2：(Aladdin reagent net, 2 μm, 99.9%)；
BN:(Mike woods, 1-2 μm, 99.9%, 99.9%)；
Cyclohexanone：(Aladdin reagent net, analysis are pure)；
Hexane：(Xi Long science limited liability company, analysis are pure)；
Hexamethylene：(Xi Long science limited liability company, analysis are pure)；
Benzene：(Xi Long science limited liability company, analysis are pure)；
Toluene：(Xi Long science limited liability company, analysis are pure)；
Dichloromethane (Sinopharm Chemical Reagent Co., Ltd., analysis are pure)；
Chloroform (Sinopharm Chemical Reagent Co., Ltd., analysis are pure)；
Dimethyl carbonate (Sinopharm Chemical Reagent Co., Ltd., analysis are pure)；
Ethyl acetate (Sinopharm Chemical Reagent Co., Ltd., analysis are pure).
Two, instrument：
Magnetic stirring apparatus：(Shandong Juancheng Chen Bo experimental facilities Co., Ltd, DHT type magnetic agitations electric jacket).
Embodiment 1：Oil-soluble fluorescent MoS2The preparation of quantum dot
(1) 150mg MoS are added to being loaded in the three-necked flask of 30ml cyclohexanone2；
(2) while magnetic stirring apparatus and electric jacket are opened, it is 140 DEG C to be heated to solution temperature under agitation, then
Constant temperature flows back 12 hours, stops stirring later, simultaneously closes off heat source, stands 3 hours；
(3) it takes supernatant liquor to centrifuge 10min at 12000r/min, collects supernatant and be put into rotary evaporator, keep
Relative degree of vacuum -40KPa is dried in vacuo 12 hours at 120 DEG C, obtains 50mg fluorescence MoS2Quantum dot.It is computed, fluorescence MoS2
The yield of quantum dot is 0.33, fluorescence quantum yield 9.6%.
Product yield calculates step：
(1) raw material MoS is weighed2Or WS2Quality is denoted as m0；
(2) the fluorescence MoS after drying is weighed2Or WS2Quantum point mass, is denoted as m1；
(3) product yield:η=m1/m0。
Fluorescence quantum yield：Fluorescence quantum yield is called fluorescence efficiency, is the build-in attribute of substance, and theoretical definition is fluorescence
The ratio between excitation light subnumber of fluorescent photon number and absorption emitted after light absorbing substance, is indicated with following formula：
Wherein Φs、ΦrIt is quantum dot and standard fluorescence substance fluorescence quantum yield to be measured, A respectivelys、ArIt indicates to wait for respectively
Substance and standard substance are surveyed in the absorbance of excitation wave strong point, Is、IrIt is illustrated respectively in test substance and mark under identical excitation wavelength
The emission peak integral area of quasi- substance.ns、nrRefractive index (the I of test substance and standard substance solvent for use is indicated respectivelys=Ir
=1.33).Using 0.1mol/L quinine sulfates sulfuric acid solution as reference substance (Φr=54%).
Fig. 1 is the transmission electron microscope picture of 1 made product of the present embodiment.Known to observation chart 1：MoS2Quantum dot monodispersity is good
It is good, particle size 4-6nm.
Fig. 3 is absorption and the fluorescent emission collection of illustrative plates that 1 made product of the present embodiment is excited using 350nm wavelength lights.Observation chart 3
Known to：The specific peak absorbance position of product is at 320nm, with typical MoS2The first absorption peak (660-680nm) phase of nanometer sheet
Than, position to shortwave direction blue shift.
Article " J phy Chem B, 1999,103:11-17. " provides following theory：Similar to MoS2Layered crystal,
Interlayer electronics confinement ability is weaker than electronics confinement ability in layer, therefore is reflected on absorption spectrum and shows as：Layered crystal ruler
Very little smaller, the position blue shift degree of the first absorption peak is bigger.
In figure 3, at 425nm, half-peak breadth is narrow, thus illustrates the present embodiment for the fluorescent emission peak position of product
Product prepared by 1 --- MoS2Concentration is compared in the grain size distribution of quantum dot.
Fig. 5 is 1 made product of the present embodiment and bulk MoS2X diffraction (XRD) comparison diagram.Known to observation chart 5：With bulk
MoS2It compares, 1 made MoS of the present embodiment2All crystallographic plane diffraction peak intensity of quantum dot are all significant lower, only in (002) crystalline substance
Face, i.e. at 2 θ=14.4 °, MoS2There is also the very small diffraction maximums of intensity for quantum dot, this shows that prepared quantum dot is size
Few layer of smaller MoS2Quantum dot.
Embodiment 2：Oil-soluble fluorescent MoS2The preparation of quantum dot
Using the method for embodiment 1, the difference is that, cyclohexanone and MoS in the present embodiment step (1)2Dosage point
It Wei not 60ml and 400mg.The embodiment is total to obtain 120mg fluorescence MoS2Quantum dot.It is computed, fluorescence MoS2The receipts of quantum dot
Rate is 0.3, fluorescence quantum yield 8.8%.
Embodiment 3：Oil-soluble fluorescent MoS2The preparation of quantum dot colloid
Take the MoS prepared in 20mg embodiments 12Quantum dot is added in 20ml hexamethylenes, ultrasonic disperse 20min, low temperature
It is kept in dark place, obtains fluorescence MoS2Quantum dot colloid.
Embodiment 4：Oil-soluble fluorescent MoS2The preparation of quantum dot colloid
Take the MoS prepared in 20mg embodiments 22Quantum dot is added in 20ml hexanes, is dispersed with stirring 20min, and low temperature is kept away
Light preserves, and obtains fluorescence MoS2Quantum dot colloid.
Embodiment 5：Oil-soluble fluorescent WS2The preparation of quantum dot
(1) 150mgWS is added to being loaded in the three-necked flask of 30ml cyclohexanone2；
(2) while magnetic stirring apparatus and electric jacket are opened, it is 140 DEG C to be heated to solution temperature under agitation, later
Constant temperature flows back 12 hours, stops stirring, simultaneously closes off heat source；
(3) solution left standstill 3 hours take supernatant liquor to centrifuge 10min at 12000r/min, collect supernatant and are put into rotation
In evaporator, relative degree of vacuum -40KPa is kept, is dried in vacuo 12 hours at 120 DEG C, obtains 45mg fluorescence WS2Quantum dot.Through
It calculates, fluorescence WS2The yield of quantum dot is 0.3, fluorescence quantum yield 6.4%.
Fig. 2 is the transmission electron microscope picture of 5 made product of the present embodiment.Known to observation chart 5：The monodispersity of made product compared with
It is good, particle size 4-6nm.
Fig. 4 is absorption and the fluorescent emission collection of illustrative plates that 5 made product of the present embodiment is excited using 350nm wavelength lights.Observation chart 4
Known to：The specific peak absorbance position of made product is at 320nm, and at 425nm, half-peak breadth compares for fluorescent emission peak position
It is narrow, illustrate WS2Quantum point grain diameter Size Distribution compares concentration.
Fig. 6 is 5 made product of the present embodiment and bulk WS2X diffraction (XRD) comparison diagram.Known to observation chart 6：With blocky WS2
It compares, 5 made WS of the present embodiment2All crystallographic plane diffraction peak intensity of quantum dot are all significant lower, only in (002) crystal face, i.e., 2
At θ=14.4 °, WS2There is also the very small diffraction maximums of intensity for quantum dot.Show that prepared quantum dot is the smaller few layer of size
Or single layer WS2Quantum dot.
Embodiment 6：Oil-soluble fluorescent WS2The preparation of quantum dot
Using the method for embodiment 5, the difference is that, cyclohexanone and WS in the present embodiment step (1)2Dosage difference
For 60ml and 400mg.The embodiment is total to obtain 100mg fluorescence WS2Quantum dot.It is computed, fluorescence MoS2The yield of quantum dot is
25.0%, fluorescence quantum yield 5.9%.
Embodiment 7：Oil-soluble fluorescent WS2The preparation of quantum dot colloid
Take the WS prepared in 20mg embodiments 52Quantum dot is added in 20ml toluene, and ultrasonic disperse 20min, low temperature is kept away
Light preserves, and obtains fluorescence WS2Quantum dot colloid.
Embodiment 8：Oil-soluble fluorescent WS2The preparation of quantum dot colloid
Take the WS prepared in 20mg embodiments 62Quantum dot is added in 20ml chloroforms, is dispersed with stirring 20min, and low temperature is kept away
Light preserves, and obtains fluorescence WS2Quantum dot colloid.
Claims (9)
1. a kind of preparation method of oil-soluble fluorescent TMDs quantum dots, which is characterized in that include the following steps：
(1) transition metal sulphur compound is added into cyclohexanone, suspension is made；
(2) suspension is carried out being heated to reflux processing, cooling and standings after reflux；
(3) it takes the supernatant liquor after standing to carry out centrifugal treating, collects the supernatant after centrifugation later and carry out rotary distillation, obtain
Oil-soluble TMDs quantum dots.
2. oil-soluble fluorescent TMDs quantum dots preparation method according to claim 1, it is characterised in that：In the step (1)
Transition metal sulphur compound is MoS2Or WS2。
3. the preparation method of oil-soluble fluorescent TMDs quantum dots according to claim 1, it is characterised in that：The step (1)
Middle transition metal sulphur compound is with cyclohexanone according to 10-400mg：The mass volume ratio of 10-100ml mixes.
4. the preparation method of oil-soluble fluorescent TMDs quantum dots according to claim 3, it is characterised in that：The step (1)
It is mixed using magnetic agitation mode, incorporation time is 8-12 minutes.
5. the preparation method of oil-soluble fluorescent TMDs quantum dots according to claim 1, it is characterised in that：The step (2)
In heating temperature be 130-140 DEG C, return time be 10-12 hour, in reflux course holding magnetic agitation state.
6. the preparation method of oil-soluble fluorescent TMDs quantum dots according to claim 1, it is characterised in that：The step (3)
In centrifuge speeds be 12000r/min, centrifugation time 10min.
7. the preparation method of oil-soluble fluorescent TMDs quantum dots according to claim 1, it is characterised in that：The step (3)
In rotary distillation condition it is as follows：Temperature is 120 DEG C, and relative degree of vacuum is -40KPa.
8. a kind of preparation method of oil-soluble fluorescent TMDs quantum dot colloids, which is characterized in that using any in claim 1-7
The oil-soluble TMDs quantum dots that method described in is prepared are scattered in nonpolar solvent, obtain oil-soluble fluorescent TMDs quantum
Point colloid.
9. the preparation method of oil-soluble fluorescent TMDs quantum dot colloids according to claim 8, which is characterized in that described non-
The one kind of polar solvent in hexane, hexamethylene, benzene, toluene, dichloromethane, chloroform, dimethyl carbonate, ethyl acetate.
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Citations (4)
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|---|---|---|---|---|
| CN103011292A (en) * | 2012-12-04 | 2013-04-03 | 北京大学 | Nolybdenum disulfide nanometer particle, preparation method and application thereof |
| CN104692463A (en) * | 2015-02-15 | 2015-06-10 | 清华大学 | Method for preparing oil-soluble nano-molybdenum disulfide |
| CN105271411A (en) * | 2015-11-04 | 2016-01-27 | 太原理工大学 | Preparation method for molybdenum disulfide quantum dot |
| CN105712404A (en) * | 2016-04-21 | 2016-06-29 | 华南师范大学 | Preparation method of MoS2 quantum dots |
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2018
- 2018-07-05 CN CN201810731510.4A patent/CN108753291B/en active Active
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| CN103011292A (en) * | 2012-12-04 | 2013-04-03 | 北京大学 | Nolybdenum disulfide nanometer particle, preparation method and application thereof |
| CN104692463A (en) * | 2015-02-15 | 2015-06-10 | 清华大学 | Method for preparing oil-soluble nano-molybdenum disulfide |
| CN105271411A (en) * | 2015-11-04 | 2016-01-27 | 太原理工大学 | Preparation method for molybdenum disulfide quantum dot |
| CN105712404A (en) * | 2016-04-21 | 2016-06-29 | 华南师范大学 | Preparation method of MoS2 quantum dots |
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