CN108046223B - Preparation method of quantum dot solution - Google Patents
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Abstract
The invention provides a preparation method of quantum dots, which comprises a femtosecond laser liquid phase ablation technology and an ultrasonic liquid phase stripping technology. Firstly, a femtosecond laser liquid phase ablation technology is adopted to crush massive multi-layer two-dimensional materials into multi-layer nano particles, and then an ultrasonic liquid phase stripping technology is adopted to strip the multi-layer nano particles into single-layer quantum dots. Other processing methods at present are that a large multi-layer two-dimensional material is firstly stripped into a single-layer large sheet, and then the large sheet is crushed into quantum dots by other means. Compared with other methods, the method has the advantages of saving time, being simple to operate and improving efficiency, and simultaneously, the method does not introduce chemical means, so that the purity of the synthesized quantum dots is high. The invention introduces a new idea for synthesizing novel nano materials and provides possibility for synthesizing controllable quantum dots.
Description
Technical Field
The invention belongs to the field of nano material preparation, and relates to a preparation method of a boron nitride or transition metal sulfide quantum dot solution.
Background
Boron Nitride (BN) and transition metal sulfides (TMDs, metal elements including molybdenum, tungsten, niobium, rhenium, titanium, chalcogens including sulfur, selenium, tellurium) are two-dimensional inorganic materials of graphene-like structure that are receiving increasing attention for their unique optical properties, high electrical conductivity, and good chemical stability. When bulk BN and TMDs materials are peeled to a single layer or few layers and the transverse dimension is reduced to be within 10nm, the materials are influenced by quantum confinement effect, present novel electronic and optical properties and become a novel quantum dot. Researches show that the BN and TMDS quantum dots have important and wide application prospects in the fields of photocatalysis, light sensing, fluorescence imaging, photothermal therapy and the like.
The current method for synthesizing BN and TMDS quantum dots mainly comprises two preparation strategies of Top-Down (Top-Down) and Bottom-Up (Bottom-Up). The top-down strategy adopts a physical and chemical method, and weakens the van der Waals force between layers by means of ultrasound, pyrolysis, electrochemistry and the like, and destroys covalent chemical bonds in the layers, thereby reducing the thickness and the transverse dimension of the sheet layer and forming a small-dimension two-dimensional quantum structure. The bottom-up strategy mainly adopts a chemical synthesis method, including a hydrothermal synthesis method, a colloid chemical method and the like. The method has the problems of complex operation, long consumed time, low production purity, non-universal method and the like, so a novel method for preparing the quantum dots, which is simple to operate, short in consumed time and high in product purity, needs to be developed.
Disclosure of Invention
The invention aims to provide a preparation method of a quantum dot solution, which is simple to operate, short in time consumption and high in quantum dot purity.
The invention is realized by the following technical scheme:
a preparation method of quantum dot solution, wherein the quantum dot is boron nitride quantum dot or transition metal sulfide quantum dot, comprises the following steps:
1) dispersing boron nitride powder or transition metal sulfide powder in an organic inert solvent, and uniformly dispersing under ultrasound to obtain a dispersion liquid;
2) under stirring, injecting femtosecond laser with the power of 200-600 mW into the dispersion liquid for ablation to obtain ablation liquid;
3) centrifuging the ablation solution to obtain supernatant;
4) and carrying out ultrasonic liquid phase stripping on the obtained supernatant to obtain the quantum dot solution.
Preferably, in step 1), the organic inert solvent is one or more of N-methylpyrrolidone, N-dimethylformamide, N-dimethylacetamide and dimethylsulfoxide.
Preferably, in the step 1), the concentration of the boron nitride powder or the transition metal sulfide powder in the dispersion liquid is 50 to 200 mg/L.
Preferably, in step 2), the total energy of the femtosecond laser injection: the mass of the boron nitride powder or the transition metal sulfide powder is 200-400 W.h/g, wherein the total energy of the femtosecond laser injection is the product of the power of the femtosecond laser and the ablation time.
Preferably, in the step 2), the stirring speed is 300-500 rpm.
Preferably, in the step 3), the time of each centrifugation is 8-12 min.
Preferably, in the step 3), the centrifugal rotating speed is 8000-12000 Xg.
Preferably, in the step 3), the ablation solution is centrifuged for 2-3 times and the supernatant is retained to obtain the supernatant.
Preferably, in step 4), the ultrasonic liquid phase stripping conditions are: the ultrasonic environment temperature is 5-15 ℃, and the ultrasonic power is 400-800 w.
Compared with the prior art, the invention has the following beneficial technical effects:
the invention provides a preparation method of quantum dot solution, which comprises the steps of firstly crushing a large-particle raw material into nano particles (multilayer nano particles) by using a femtosecond laser ablation method, and further stripping the nano particles into single-layer or few-layer quantum dots in a short time by using an ultrasonic liquid phase stripping technology; the method of the invention uses few chemical reagents, so the produced quantum dots have higher purity and the chemical pollution is reduced. Compared with the traditional method, the method provided by the invention has the advantages of simple operation, short time consumption and high quantum dot purity.
Drawings
FIG. 1 is a transmission electron microscopic image and a high resolution transmission electron microscopic image of boron nitride quantum dots prepared by the method of the present invention.
Fig. 2-1 is an atomic force microscopic image of boron nitride quantum dots prepared by the method of the present invention.
Fig. 2-2 is a profile height distribution of boron nitride quantum dots prepared by the method of the present invention.
FIG. 3 shows Raman spectra of bulk hexagonal boron nitride and boron nitride quantum dots prepared by the method of the present invention.
FIG. 4 is a photoluminescence spectrum of boron nitride quantum dots prepared by the method of the present invention.
FIG. 5 shows MoS2TEM (transmission electron microscope) results of the quantum dots.
FIG. 6 shows WS2TEM (transmission electron microscope) results of the quantum dots.
Detailed Description
The present invention will now be described in further detail with reference to specific examples, which are intended to be illustrative, but not limiting, of the invention.
Example 1
1) Bulk BN material was milled to a small particle powder and 50mg of the powder was dispersed in 5mL of N-methylpyrrolidone (NMP) solution and sonicated at 300W for 2-3min to disperse uniformly. And taking out 300 mu L of the dispersed sample, putting the sample in 40mL of N-methylpyrrolidone (NMP) solution again, and carrying out ultrasonic treatment for 2-3min at the power of 300W to uniformly disperse the sample to obtain a dispersion liquid.
2) 10mL of the prepared dispersion liquid is placed in a 10mL beaker, a magnetic rotor is placed in the beaker, the beaker is placed on a magnetic stirrer, stirring is carried out at the rotating speed of 400 r/min, and simultaneously, a femtosecond laser with the power of 400mW is injected into the beaker for ablation.
3) After 30min of ablation, the liquid is changed from a transparent state to light yellow, the sample synthesized by ablation is centrifuged to remove unreacted or incompletely reacted large particles, the centrifugal acceleration is 10800 Xg, the centrifugation time is 10min, and the steps are repeated twice.
4) The supernatant after centrifugation was removed and stored in a 50 ml centrifuge tube. The four supernatants were combined (40 mL of dispersion was prepared in step 1 and treated as 10mL batches).
5) And (3) putting 20-30mL of the supernatant into a constant-temperature ultrasonic crusher for ultrasonic liquid phase stripping, wherein the ultrasonic environment temperature is set to be 10 ℃, the ultrasonic power is 600W, and the ultrasonic time is 2 h.
6) And after the ultrasonic liquid phase stripping is finished, taking out the sample, and storing the sample in a cool and ventilated place to obtain the quantum dot solution.
Example 2
1) The block body MoS2The material was milled to a small particle powder and 50mg of the powder was dispersed in 5mL of N, N-Dimethylformamide (DMF) solution and sonicated at 350W for 2-3min to disperse uniformly. And taking 300 mu L of the dispersed sample out, putting the sample in 40mL of DMF solution again, and carrying out ultrasonic treatment for 2-3min by adopting 300W power to uniformly disperse the sample to obtain a dispersion liquid.
2) 10mL of the prepared dispersion liquid is placed in a 10mL beaker, a magnetic rotor is placed in the beaker, the beaker is placed on a magnetic stirrer, stirring is carried out at the rotating speed of 500 r/min, and simultaneously, laser with the power of 600mW is injected into the beaker for ablation.
3) After 90min of ablation, the liquid is changed from a transparent state to light yellow, the sample synthesized by ablation is centrifuged to remove unreacted or incompletely reacted large particles, the centrifugal acceleration is 8000 Xg, the centrifugation time is 10min, and the steps are repeated twice.
4) The supernatant after centrifugation was removed and stored in a 50 ml centrifuge tube. The four supernatants were combined (40 mL of dispersion was prepared in step 1).
5) And putting the supernatant into a constant-temperature ultrasonic crusher for ultrasonic liquid phase stripping, wherein the ultrasonic environment temperature is set to be 20 ℃, the ultrasonic power is 700W, and the ultrasonic time is 2.5 h.
6) And after the ultrasonic liquid phase stripping is finished, taking out the sample, and storing the sample in a cool and ventilated place.
MoS2The TEM results of the quantum dots are shown in fig. 5.
Example 3
1) Block WS2Grinding the material into small particle powder, dispersing 50mg of the powder in 10mL of N, N-Dimethylformamide (DMF) solution, and performing ultrasonic treatment with 400W power for 2-3min to uniformly disperse the powder to obtain a dispersion liquid. After being dispersedTaking out 200 mu L of the sample, putting the sample in 40mL of DMF solution again, and carrying out ultrasonic treatment for 2-3min by adopting 400W power to uniformly disperse the sample to obtain a dispersion liquid.
2) 10mL of the prepared dispersion liquid is placed in a 10mL beaker, a magnetic rotor is placed in the beaker, the beaker is placed on a magnetic stirrer, stirring is carried out at the rotating speed of 400 r/min, and simultaneously, a laser with the power of 500mW is injected into the beaker for ablation.
3) After ablation for 18min, the liquid turns from transparent state to light yellow, and the sample synthesized by ablation is centrifuged to remove unreacted or incompletely reacted large particles, the centrifugation acceleration is 12000 Xg, the centrifugation time is 12min, and the steps are repeated twice.
4) The supernatant after centrifugation was removed and stored in a 50 ml centrifuge tube. The four supernatants were combined (40 mL of dispersion was prepared in step 1).
5) And putting the supernatant into a constant-temperature ultrasonic crusher for ultrasonic liquid phase stripping, wherein the ultrasonic environment temperature is set to be 15 ℃, the ultrasonic power is 800W, and the ultrasonic time is 2 h.
6) And after the ultrasonic liquid phase stripping is finished, taking out the sample, and storing the sample in a cool and ventilated place.
WS2The TEM results of the quantum dots are shown in fig. 6.
Example 4
1) The block body MoSe2Grinding the material into small particle powder, dispersing 100mg of the powder in 5mL of N, N-Dimethylacetamide (DMA) solution, performing ultrasonic treatment at 500W for 2-3min to uniformly disperse the powder, taking 400 mu L of the dispersed sample out, placing the sample in 40mL of DMA solution again, and performing ultrasonic treatment at 400W for 2-3min to uniformly disperse the sample to obtain a dispersion liquid.
2) 10mL of the prepared dispersion liquid is placed in a 10mL beaker, a magnetic rotor is placed in the beaker, the beaker is placed on a magnetic stirrer, stirring is carried out at the rotating speed of 300 r/min, and simultaneously, laser with the power of 200mW femtosecond is injected into the beaker for ablation.
3) And after ablation for 3h, the liquid is changed from a transparent state to light yellow, the sample synthesized by ablation is centrifuged to remove unreacted or incompletely reacted large particles, the centrifugation acceleration is 11000 Xg, the centrifugation time is 8min, and the steps are repeated for three times.
4) The supernatant after centrifugation was taken out and stored in a 10ml centrifuge tube. The four supernatants were combined (40 mL of dispersion was prepared in step 1).
5) And putting the supernatant into a constant-temperature ultrasonic crusher for ultrasonic liquid phase stripping, wherein the ultrasonic environment temperature is set to be 5 ℃, the ultrasonic power is 800W, and the ultrasonic time is 1.5 h.
6) And after the ultrasonic liquid phase stripping is finished, taking out the sample, and storing the sample in a cool and ventilated place.
Example 5
1) WSe the block2Grinding the material into small particle powder, dispersing 50mg of the powder in 10mL of dimethyl sulfoxide (DMSO) solution, performing ultrasonic treatment at 600W for 2-3min to uniformly disperse the powder, taking out 1000 mu L of the dispersed sample, placing the sample in 40mL of DMA solution again, and performing ultrasonic treatment at 400W for 2-3min to uniformly disperse the sample to obtain a dispersion liquid.
2) 10mL of the prepared dispersion liquid is placed in a 10mL beaker, a magnetic rotor is placed in the beaker, the beaker is placed on a magnetic stirrer, stirring is carried out at the rotating speed of 500 r/min, and simultaneously, laser with the power of 600mW is injected into the beaker for ablation.
3) After ablation for 80min, the liquid turns from transparent state to light yellow, the sample synthesized by ablation is centrifuged to remove unreacted or incompletely reacted large particles, the centrifugal acceleration is 9000 Xg, the centrifugation time is 10min, and the steps are repeated twice.
4) The supernatant after centrifugation was removed and stored in a 50 ml centrifuge tube. The four supernatants were combined (40 mL of dispersion was prepared in step 1).
5) And putting the supernatant into a constant-temperature ultrasonic crusher for ultrasonic liquid phase stripping, wherein the ultrasonic environment temperature is set to be 10 ℃, the ultrasonic power is 800W, and the ultrasonic time is 1.5 h.
6) And after the ultrasonic liquid phase stripping is finished, taking out the sample, and storing the sample in a cool and ventilated place.
Example 6
The boron nitride quantum dots synthesized in example 1 were subjected to transmission electron microscopy (results are shown in fig. 1), atomic force microscopy (results are shown in fig. 2-1 and 2-2), raman spectroscopy (results are shown in fig. 3), and photoluminescence spectra thereof were detected (results are shown in fig. 4).
As shown in fig. 1, the transmission electron microscopy image shows that the synthesized quantum dots are uniformly distributed without any cluster, and the high-resolution transmission electron microscopy image shows that the lattice spacing of the quantum dots is 0.22cm, which indicates that the synthesized quantum dots are boron nitride corresponding to the (100) crystal plane of boron nitride.
As shown in fig. 2-1 and 2-2, the atomic force microscopy images of the quantum dots and the profile heights thereof indicate that the height of the synthesized boron nitride quantum dots is about 1-2nm, and the quantum dots have a single-layer or few-layer structure.
Raman spectra of hexagonal boron nitride (h BN Powder) and Boron Nitride Quantum Dots (BNQDs) are shown in FIG. 3, both materials at 1376cm-1A clear Raman peak exists at all, which indicates that the boron nitride quantum dots synthesized by the method still maintain the B-N structure, and the method does not damage the structure of the boron nitride.
FIG. 4 shows photoluminescence spectra of boron nitride quantum dots, which can be observed to have an obvious fluorescence emission peak in a 400nm-500nm band, and prove that the nano material synthesized by the method of the invention has strong fluorescence characteristics and can be used as a fluorescence probe for biological imaging and biological sensing.
The invention provides a preparation method of quantum dots, which comprises a femtosecond laser liquid phase ablation technology and an ultrasonic liquid phase stripping technology. Firstly, a femtosecond laser liquid phase ablation technology is adopted to crush massive multi-layer two-dimensional materials into multi-layer nano particles, and then an ultrasonic liquid phase stripping technology is adopted to strip the multi-layer nano particles into single-layer quantum dots. Other processing methods at present are that a large multi-layer two-dimensional material is firstly stripped into a single-layer large sheet, and then the large sheet is crushed into quantum dots by other means. Compared with other methods, the method has the advantages of saving time, being simple to operate and improving efficiency, and simultaneously, the method does not introduce chemical means, so that the purity of the synthesized quantum dots is high. The invention introduces a new idea for synthesizing novel nano materials and provides possibility for synthesizing controllable quantum dots.
Claims (5)
1. A preparation method of a quantum dot solution, wherein the quantum dot is a boron nitride quantum dot, and is characterized by comprising the following steps:
1) dispersing boron nitride powder in an organic inert solvent, and uniformly dispersing under ultrasound to obtain a dispersion liquid;
the organic inert solvent is one or more of N-methyl pyrrolidone, N-dimethylformamide, N-dimethylacetamide and dimethyl sulfoxide;
2) under stirring, injecting femtosecond laser with the power of 200-600 mW into the dispersion liquid for ablation to obtain ablation liquid;
total energy of femtosecond laser injection: the mass of the boron nitride powder is = 200-1200 W.h/g, wherein the total energy injected by the femtosecond laser is the product of the power of the femtosecond laser and the ablation time;
the stirring speed is 300-500 r/min;
3) centrifuging the ablation solution to obtain supernatant;
4) carrying out ultrasonic liquid phase stripping on the obtained supernatant to obtain a quantum dot solution;
the ultrasonic liquid phase stripping conditions are as follows: the ultrasonic environment temperature is 5-20 ℃, and the ultrasonic power is 400-800 w;
the lattice spacing of the quantum dots is 0.22nm, the height of the quantum dots is about 1-2nm, and the quantum dots have a single-layer or few-layer structure.
2. The method for preparing a quantum dot solution according to claim 1, wherein in the step 1), the concentration of the boron nitride powder in the dispersion is 50 to 200 mg/L.
3. The method for preparing a quantum dot solution according to claim 1, wherein in the step 3), the time for each centrifugation is 8-12 min.
4. The method for preparing a quantum dot solution according to claim 1, wherein in the step 3), the centrifugal rotation speed is 8000 to 12000 Xg.
5. The method for preparing the quantum dot solution according to claim 1, wherein in the step 3), the ablative solution is centrifuged 2-3 times and the supernatant is retained to obtain the supernatant.
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| CN108906013B (en) * | 2018-07-23 | 2021-09-14 | 合肥工业大学 | Method for preparing titanium dioxide quantum dots through ultrasonic crushing |
| CN109317183B (en) * | 2018-11-12 | 2020-06-12 | 湖南大学 | Boron nitride quantum dot/ultrathin porous carbon nitride composite photocatalytic material and preparation method and application thereof |
| CN109399724A (en) * | 2018-11-26 | 2019-03-01 | 深圳大学 | The preparation method of rhenium disulfide quantum dot |
| CN110092359B (en) * | 2019-05-27 | 2022-08-09 | 华东师范大学 | Method for preparing vanadium diselenide quantum dots through liquid phase stripping |
| CN110272048B (en) * | 2019-06-17 | 2022-04-22 | 西安电子科技大学 | Preparation method of two-dimensional layered nano material MXene quantum dots |
| CN110194464B (en) * | 2019-06-25 | 2022-06-07 | 中北大学 | Preparation method and application of boron quantum dots |
| CN113697822B (en) * | 2020-05-20 | 2022-11-29 | 中国科学院理化技术研究所 | Boron quantum dot and preparation method and application thereof |
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