CN108753291B - Oil-soluble fluorescent TMDS quantum dot and preparation method of colloid thereof - Google Patents
Oil-soluble fluorescent TMDS quantum dot and preparation method of colloid thereof Download PDFInfo
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- CN108753291B CN108753291B CN201810731510.4A CN201810731510A CN108753291B CN 108753291 B CN108753291 B CN 108753291B CN 201810731510 A CN201810731510 A CN 201810731510A CN 108753291 B CN108753291 B CN 108753291B
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Abstract
The invention relates to the technical field of nano material preparation, in particular to a preparation method of oil-soluble fluorescent TMDs quantum dots and colloid thereof; comprises (1) adding transition metal sulfur compound into cyclohexanone to obtain suspension; (2) heating and refluxing the suspension, and cooling and standing after refluxing; (3) and centrifuging the supernatant after standing, collecting the centrifuged supernatant, and performing rotary distillation to obtain the oil-soluble TMDS quantum dots. The invention has the beneficial effects that: the method is simple, the conditions are mild and safe, the equipment cost is low, the preparation efficiency is high, and the post purification treatment is not needed.
Description
Technical Field
The invention relates to the technical field of nano material preparation, in particular to a preparation method of an oil-soluble fluorescent TMDs quantum dot and a colloid thereof.
Background
Quantum Dots (QDs) are zero-dimensional nano semiconductor materials, have a series of unique photoelectric properties, and are widely applied to the fields of solar cells, luminescent devices, biomedicine and the like. Two-dimensional transition metal chalcogenides (TMDs) refer to X-M-X type sandwich compounds formed of a transition metal element (M) and a chalcogen nonmetal element (X), such as MoS2、WS2And the like. TMDs research has been focused on the micro and nano scale for a long time. As materials technology developed, it was discovered that by further reducing the material size, MoS2、WS2The material with direct band gap can be mutated from indirect band gap, and has physical and chemical properties, such as high fluorescence quantum yield, extinction coefficient, and resistance to bleachingPoise capacity, wide excitation spectrum range, ultrahigh electron transfer rate and the like. Can be applied to the fields of fluorescent ink, photoelectric devices, biological markers, fluorescent probes and the like.
The base material of the existing fluorescent electronic material ink mainly comprises II-VI group quantum dots, such as CdSe, CdSe/CdS and the like, wherein cadmium and other harmful heavy metals are not beneficial to environmental protection. In addition, the preparation of the II-VI quantum dots with the emission wavelength of 400-500nm is quite difficult. And MoS2、WS2The quantum dot emission spectrum regions overlap with this range exactly.
Thus, preparation of oil-soluble fluorescent MoS2、WS2The quantum dot pair has important significance for preparing fluorescent electronic material ink.
Currently, oil-soluble fluorescent MoS2、WS2The preparation of quantum dots mainly adopts a solvothermal method, a thermal injection method and the like, and the currently disclosed scheme is as follows:
1) hongtao et al (Inorganic Chemistry,2008,47, (5):1428-2And (4) quantum dots.
2) Claudia Altavilla et al (Chemistry of materials,2011,23(17):3879-4)2MoS4As a precursor, oleylamine as a solvent, MoS was obtained at high temperature2And WS2And (4) quantum dots.
3) Yueli Liu et al (Journal of Materials Science: Materials in Electronics,2017,28(18): 13633-2And (4) quantum dots.
In each scheme, although oil-soluble TMDs quantum dots and colloids thereof can be obtained, the quantum dot synthesis process involves a large amount of toxic solvents, the process requirements are strict, if high temperature, anhydrous and oxygen-free environments and the like are required, the types of selectable precursors are limited. The late purification process of the product is complex, and the yield is low.
Therefore, the development of a simple and effective method for preparing the fluorescent transition metal sulfide quantum dots with oil solubility and high fluorescent quantum dot yield is urgently needed.
Disclosure of Invention
The technical problem to be solved by the invention is that the existing preparation method of the oil-soluble fluorescent TMDs quantum dot is complex and unsafe.
In order to solve the technical problems, the technical scheme adopted by the invention is as follows: a preparation method of oil-soluble fluorescent TMDs quantum dots comprises the following steps:
(1) adding a transition metal sulfur compound into cyclohexanone to prepare a suspension;
(2) heating and refluxing the suspension, and cooling and standing after refluxing;
(3) and centrifuging the supernatant after standing, collecting the centrifuged supernatant, and performing rotary distillation to obtain the oil-soluble TMDS quantum dots.
The solubility of nanomaterials in solvents can be described by hansen solubility parameter theory (HSP). I.e. the smaller the dispersion force, permanent dipole force, hydrogen bond difference of the nanomaterial and the solvent, the greater its solubility in the solvent. The concrete formula is as follows:
wherein, deltaD,sol、δP,sol、δH,solSolvent dispersion forces, permanent dipole forces, hydrogen bonding, respectively. DeltaD,NS、δP,NS、δH,NSRespectively nanoparticle dispersion force, permanent dipole force, hydrogen bonding. RaThe smaller the value, the greater the solubility of the nanomaterial in the solvent. MoS2The dispersion force, permanent dipole force, and hydrogen bond are: 17-19MPa0.5,6-12MPa0.5,4.5-8.4MPa0.5。WS2The dispersion force, permanent dipole force, and hydrogen bond are: 16-18MPa0.5,5-14MPa0.5,2-19MPa0.5。
In the above technical scheme, the dispersion force, permanent dipole force and hydrogen bond of the selected solvent cyclohexanone are respectively: 17.2MPa0.5,10.6MPa0.5,4.8MPa0.5And MoS2，WS2The corresponding parameter values are very close. Thus, MoS2、WS2Etc. have higher solubility in cyclohexanone. Stripping MoS by using cyclohexanone as solvent through simple heating reflux method2、WS2Etc., higher yields of MoS can be obtained2、WS2And (4) quantum dots.
Further, the transition metal sulfur compound in the step (1) is MoS2、WS2And the like.
Further, the transition metal sulfur compound and cyclohexanone in the step (1) are mixed according to a ratio of 10-400 mg: mixing at a mass-to-volume ratio of 10-100 ml.
Further, the step (1) adopts a magnetic stirring mode to mix for 8-12 minutes.
Further, the heating temperature in the step (2) is 130-140 ℃, the reflux time is 10-12 hours, and the magnetic stirring state is maintained during the reflux process.
Further, the centrifugal separation speed in the step (3) is 12000r/min, and the centrifugal time is 10 min.
Further, the rotary distillation conditions in the step (3) are as follows: the temperature was 120 ℃ and the relative vacuum was-40 KPa.
The invention also aims to provide a preparation method of the oil-soluble fluorescent TMDs quantum dot colloid, wherein the oil-soluble TMDs quantum dot prepared by the method is dispersed in a nonpolar solvent to obtain the oil-soluble fluorescent TMDs quantum dot colloid.
The non-polar solvent includes, but is not limited to, hexane, cyclohexane, benzene, toluene, dichloromethane, chloroform, dimethyl carbonate, or ethyl acetate.
The invention has the beneficial effects that: the method is simple, the conditions are mild and safe, the equipment cost is low, the preparation efficiency is high, and the post purification treatment is not needed.
Drawings
FIG. 1 is a transmission electron micrograph of a product prepared in example 1 of the present invention;
FIG. 2 is a transmission electron micrograph of a product prepared in example 5 of the present invention;
FIG. 3 is an absorption and fluorescence emission spectrum of a product prepared in example 1 of the present invention;
FIG. 4 is an absorption and fluorescence emission spectrum of a product prepared in example 5 of the present invention;
FIG. 5 is an X-ray diffraction pattern of the product prepared in example 1 of the present invention;
FIG. 6 is an X-ray diffraction pattern of the product prepared in example 5 of the present invention.
Detailed Description
The invention is further illustrated below in conjunction with examples 1-8, in which the reagents and instrumentation are derived from the following sources:
firstly, a reagent:
MoS2: purchased from Zhengzhou Jinshan chemical Co., Ltd., 44 μm, 99.9%);
WS2: (Aladdin reagent net, 2 μm, 99.9%);
BN (Mecline, 1-2 μm, 99.9%, 99.9%);
cyclohexanone: (Aladdin reagent net, analytical grade);
hexane: (Xiong science corporation, analytical purity);
cyclohexane: (Xiong science corporation, analytical purity);
benzene: (Xiong science corporation, analytical purity);
toluene: (Xiong science corporation, analytical purity);
dichloromethane (chemical reagent of national drug group, chemical reagent limited, analytical purity);
chloroform (chemical reagent, Inc., analytical purity of national drug group);
dimethyl carbonate (chemical reagent of national drug group, chemical reagent of limited company, analytical purity);
ethyl acetate (chemical reagent of national drug group, ltd., analytical purity).
II, an instrument:
a magnetic stirrer: (Juancheng Shandong Chenbo laboratory equipment Co., Ltd., DHT type magnetic stirring electric jacket).
Example 1: oil-soluble fluorescent MoS2Preparation of quantum dots
(1) To a tri-phase solution containing 30ml of cyclohexanone150mg MoS is added into a flask with a mouth2；
(2) Simultaneously starting a magnetic stirrer and an electric heating sleeve, heating to 140 ℃ under the stirring condition, refluxing at constant temperature for 12 hours, stopping stirring, simultaneously closing a heat source, and standing for 3 hours;
(3) centrifuging the supernatant at 12000r/min for 10min, collecting supernatant, placing into rotary evaporator, maintaining relative vacuum degree of-40 KPa, and vacuum drying at 120 deg.C for 12 hr to obtain 50mg fluorescent MoS2And (4) quantum dots. Calculated, fluorescent MoS2The yield of quantum dots was 0.33 and the fluorescence quantum yield was 9.6%.
And (3) calculating the product yield:
(1) weighing raw material MoS2Or WS2Mass, is recorded as m0；
(2) Weighing dried fluorescent MoS2Or WS2Mass of quantum dots, denoted m1；
(3) The product yield is eta ═ m1/m0。
Fluorescence quantum yield: the fluorescence quantum yield, also called fluorescence efficiency, is an intrinsic property of a substance, and is theoretically defined as the ratio of the number of fluorescence photons emitted by a fluorescent substance after absorption of light to the number of excitation light photons absorbed, and is expressed by the following formula:
wherein phis、ΦrRespectively the fluorescence quantum yield of the quantum dot to be detected and the standard fluorescent substance, As、ArRespectively represents the absorbance of the substance to be measured and the standard substance at the excitation wavelength, Is、IrThe integrated areas of the emission peaks of the test substance and the standard substance at the same excitation wavelength are respectively shown. n iss、nrRespectively, the refractive indices (I) of the solvents used for the test substance and the standard substances＝Ir1.33). 0.1mol/L quinine sulfate solution is used as a standard substance (phi)r＝54％)。
FIG. 1 shows the product obtained in example 1Transmission electron micrographs of the object. As can be seen from the observation of FIG. 1: MoS2The quantum dots have good monodispersity and the particle size of 4-6 nm.
FIG. 3 is an absorption and fluorescence emission spectrum of the product prepared in this example 1 excited with a 350nm wavelength light. As can be seen from fig. 3: the characteristic peak absorption position of the product is at 320nm, and the product is similar to the typical MoS2The position of the first absorption peak (660-680nm) of the nano-sheet is blue-shifted towards the short wave direction.
The article "J phy Chem B,1999,103: 11-17" gives the following theory: similar to MoS2Layered crystals, which have weaker interlayer electron confinement than intralayer electron confinement, therefore appear as reflected in the absorption spectrum: the smaller the size of the layered crystal, the greater the degree of blue shift of the position of the first absorption peak thereof.
In FIG. 3, the fluorescence emission peak of the product was at 425nm, and the half-width thereof was relatively narrow, thereby illustrating that MoS was the product prepared in example 12The particle size distribution of the quantum dots is concentrated.
FIG. 5 shows the product and the bulk MoS obtained in example 12X-ray diffraction (XRD) contrast pattern of (c). As can be seen from fig. 5: with massive MoS2In contrast, the MoS made in example 12The diffraction peak intensity of all crystal planes of the quantum dot is obviously low, and MoS is only formed in a (002) crystal plane, namely a 2 theta 14.4 DEG position2The quantum dots also have diffraction peaks with very small intensity, which indicates that the prepared quantum dots are few-layer MoS with smaller size2And (4) quantum dots.
Example 2: oil-soluble fluorescent MoS2Preparation of quantum dots
The method of example 1 was used except that cyclohexanone and MoS were present in step (1) of this example2The amounts used were 60ml and 400mg, respectively. This example gives a total of 120mg of fluorescent MoS2And (4) quantum dots. Calculated, fluorescent MoS2The yield of quantum dots was 0.3 and the yield of fluorescent quantum dots was 8.8%.
Example 3: oil-soluble fluorescent MoS2Preparation of Quantum dot colloids
20mg of the MoS prepared in example 1 were taken2Quantum dots, added into 20ml cyclohexane, dispersed by ultrasound 2Storing at low temperature in dark for 0min to obtain fluorescent MoS2And (3) quantum dot colloid.
Example 4: oil-soluble fluorescent MoS2Preparation of Quantum dot colloids
20mg of MoS prepared in example 2 were taken2Adding quantum dots into 20ml of hexane, stirring and dispersing for 20min, and storing at low temperature in the dark to obtain the fluorescent MoS2And (3) quantum dot colloid.
Example 5: oil soluble fluorescent WS2Preparation of quantum dots
(1) Into a three-necked flask containing 30ml of cyclohexanone, 150mgWS was charged2；
(2) Simultaneously starting a magnetic stirrer and an electric heating sleeve, heating to 140 ℃ under the stirring condition, then refluxing at constant temperature for 12 hours, stopping stirring, and simultaneously closing a heat source;
(3) standing the solution for 3 hr, centrifuging supernatant at 12000r/min for 10min, collecting supernatant, placing into rotary evaporator, maintaining relative vacuum degree of-40 KPa, and vacuum drying at 120 deg.C for 12 hr to obtain 45mg fluorescent WS2And (4) quantum dots. Calculated, fluorescence WS2The yield of quantum dots was 0.3 and the yield of fluorescent quantum dots was 6.4%.
FIG. 2 is a transmission electron micrograph of the product obtained in example 5. As can be seen from fig. 5: the prepared product has better monodispersity and the particle size is 4-6 nm.
FIG. 4 is an absorption and fluorescence emission spectrum of the product prepared in this example 5 excited with a 350nm wavelength light. As can be seen from fig. 4: the characteristic peak absorption position of the prepared product is at 320nm, the fluorescence emission peak position is at 425nm, the half-peak width is narrow, and WS is shown2The particle size distribution of the quantum dots is concentrated.
FIG. 6 shows the product and the bulk WS obtained in example 52X-ray diffraction (XRD) contrast pattern. As can be seen from fig. 6: and block WS2In contrast, WS produced in example 52All the crystal planes of the quantum dots have obviously low diffraction peak intensity, and WS is only in (002) crystal planes, namely 2 theta is 14.4 degrees2Quantum dots also have diffraction peaks with very small intensities. Indicating that the prepared quantum dots are few layers or single layer WS with smaller size2Quantum dots。
Example 6: oil soluble fluorescent WS2Preparation of quantum dots
The process of example 5 was used except that cyclohexanone and WS were used in step (1) of this example2The amounts used were 60ml and 400mg, respectively. This example gives 100mg of fluorescent WS in total2And (4) quantum dots. Calculated, fluorescent MoS2The yield of the quantum dots is 25.0%, and the yield of the fluorescence quantum dots is 5.9%.
Example 7: oil soluble fluorescent WS2Preparation of Quantum dot colloids
20mg of WS prepared in example 5 were taken2Adding quantum dots into 20ml toluene, ultrasonic dispersing for 20min, storing at low temperature in dark to obtain fluorescent WS2And (3) quantum dot colloid.
Example 8: oil soluble fluorescent WS2Preparation of Quantum dot colloids
20mg of WS prepared in example 6 were taken2Adding quantum dots into 20ml chloroform, stirring and dispersing for 20min, storing at low temperature in dark place to obtain fluorescent WS2And (3) quantum dot colloid.
Claims (6)
1. A preparation method of oil-soluble fluorescent TMDs quantum dots is characterized by comprising the following steps:
(1) adding a transition metal sulfur compound into cyclohexanone to prepare a suspension; the transition metal sulfur compound is MoS2Or WS2(ii) a The transition metal sulfur compound and cyclohexanone are mixed according to a weight ratio of 10-400 mg: mixing 10-100ml in a mass-to-volume ratio;
(2) heating and refluxing the suspension, and cooling and standing after refluxing; the heating temperature is 130-140 ℃, the reflux time is 10-12 hours, and the magnetic stirring state is kept in the reflux process
(3) And centrifuging the supernatant after standing, collecting the centrifuged supernatant, and performing rotary distillation to obtain the oil-soluble TMDS quantum dots.
2. The method for preparing the oil-soluble fluorescent TMDs quantum dot according to claim 1, wherein: and (2) mixing in the step (1) in a magnetic stirring manner for 8-12 minutes.
3. The method for preparing the oil-soluble fluorescent TMDs quantum dot according to claim 1, wherein: the centrifugal separation speed in the step (3) is 12000r/min, and the centrifugal time is 10 min.
4. The method for preparing the oil-soluble fluorescent TMDs quantum dot according to claim 1, wherein: the rotary distillation conditions in the step (3) are as follows: the temperature was 120 ℃ and the relative vacuum was-40 KPa.
5. A preparation method of oil-soluble fluorescent TMDs quantum dot colloid is characterized in that the oil-soluble TMDs quantum dot prepared by the method of any one of claims 1 to 4 is dispersed in a non-polar solvent to obtain the oil-soluble fluorescent TMDs quantum dot colloid.
6. The method for preparing the oil-soluble fluorescent TMDs quantum dot colloid of claim 5, wherein the non-polar solvent is selected from one of hexane, cyclohexane, benzene, toluene, dichloromethane, chloroform, dimethyl carbonate, and ethyl acetate.
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| 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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| 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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