CN108046223A - A kind of preparation method of quantum dot solution - Google Patents
A kind of preparation method of quantum dot solution Download PDFInfo
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- CN108046223A CN108046223A CN201810078189.4A CN201810078189A CN108046223A CN 108046223 A CN108046223 A CN 108046223A CN 201810078189 A CN201810078189 A CN 201810078189A CN 108046223 A CN108046223 A CN 108046223A
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B21/00—Nitrogen; Compounds thereof
- C01B21/06—Binary compounds of nitrogen with metals, with silicon, or with boron, or with carbon, i.e. nitrides; Compounds of nitrogen with more than one metal, silicon or boron
- C01B21/064—Binary compounds of nitrogen with metals, with silicon, or with boron, or with carbon, i.e. nitrides; Compounds of nitrogen with more than one metal, silicon or boron with boron
- C01B21/0648—After-treatment, e.g. grinding, purification
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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
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- C01G39/06—Sulfides
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- C01P2006/60—Optical properties, e.g. expressed in CIELAB-values
Abstract
The present invention proposes a kind of preparation method of quantum dot, including two parts of femtosecond laser liquid phase ablation technology and ultrasonic liquid-phase lift-off technology.The two-dimensional material crushing of bulk multilayer is the nano particle of multilayer by femtosecond laser liquid phase ablation technology first, then the nano particle of multilayer is removed to the quantum dot into individual layer using ultrasonic liquid-phase lift-off technology.And other processing methods are first to remove bulk multilayer two-dimension material into individual layer sheet at present, then be aided with other means and crush sheet for quantum dot.The advantages of present invention has compared with other methods and saves the time, easy to operate, raising efficiency, while because the invention does not introduce chemical means, therefore the quantum dot purity synthesized is high.The present invention introduces new thinking for synthesizing new nano material, and provides possibility to synthesize regulatable quantum dot.
Description
Technical field
The invention belongs to field of nano material preparation, it is related to a kind of boron nitride or transient metal sulfide quantum dot solution
Preparation method.
Background technology
(TMDs, metallic element include molybdenum, tungsten, niobium, rhenium, titanium, chalcogen bag for boron nitride (BN) and transient metal sulfide
Include sulphur, selenium, tellurium) be similar graphene-structured Two-dimensional Inorganic material, because of its unique optical characteristics, high conductivity and good
Chemical stability receives more and more attention.When block BN and TMDs material is stripped to individual layer or few layer, and its horizontal ruler
Very little when being decreased within 10nm, material is influenced by quantum confined effect, is showed novel electronics and optical property, is become one
The new quantum dot of class.Research shows BN and TMDs quantum dots in necks such as photocatalysis, light sensing, fluorescence imaging and photo-thermal therapies
Domain has important and wide application prospect.
The method of synthesis BN and TMDs quantum dots mainly includes (Top-Down) and from bottom to top from top to bottom at present
(Bottom-Up) strategy is prepared for two kinds.Top-down strategy uses physicochemical method, passes through ultrasound, pyrolysis and electrification
Etc. means weaken the Van der Waals force of interlayer, destroy the covalent chemical bond in layer, so as to reduce the thickness of lamella and lateral dimension,
Form the two-dimentional quantum structure of small size.Strategy from bottom to top mainly using the method for chemical synthesis, is closed including hydro-thermal
Into method and colloid chemistry methods etc..Above method there is it is complicated for operation, time-consuming, production purity it is low, method is not general the problems such as,
Therefore need to develop a kind of quantum dot novel preparation method short, product purity is high easy to operate, time-consuming.
The content of the invention
It is easy to operate it is an object of the invention to provide a kind of preparation method of quantum dot solution, take short, quantum dot
Purity is high.
The present invention is to be achieved through the following technical solutions：
A kind of preparation method of quantum dot solution, the quantum dot are boron nitride quantum dot or transient metal sulfide quantum
Point, including step：
1) boron nitride powder or transient metal sulfide powder are dispersed in organic inert solvent, and disperseed under ultrasound
Uniformly, dispersion liquid is obtained；
2) ablation is carried out in the femtosecond laser for being under stiring, 200mW~600mW with power injection dispersion liquid, is burnt
Lose liquid；
3) ablation liquid obtains supernatant by centrifuging；
4) gained supernatant is subjected to ultrasonic liquid-phase stripping, obtains quantum dot solution.
Preferably, in step 1), the organic inert solvent for N-Methyl pyrrolidone, n,N-Dimethylformamide,
One or more in DMAC N,N' dimethyl acetamide, dimethyl sulfoxide (DMSO).
Preferably, in step 1), in dispersion liquid, the concentration of boron nitride powder or transient metal sulfide powder for 50~
200mg/L。
Preferably, in step 2), the gross energy of femtosecond laser injection：Boron nitride powder or transient metal sulfide powder
Quality=200~400Wh/g, wherein, the gross energy of femtosecond laser injection is power and the ablation time of femtosecond laser
Product.
Preferably, in step 2), the speed of stirring is 300~500 turns/min.
Preferably, in step 3), the time centrifuged every time is 8~12min.
Preferably, in step 3), centrifugal rotational speed is 8000~12000 × g.
Preferably, in step 3), ablation liquid repeats 2~3 operations for centrifuging and retaining supernatant, obtains supernatant.
Preferably, in step 4), the condition that ultrasonic liquid-phase is removed is：Ultrasound environments temperature is 5~15 DEG C, ultrasonic power
For 400~800w.
Compared with prior art, the present invention has technique effect beneficial below：
The present invention proposes a kind of preparation method of quantum dot solution, first using the method for femtosecond laser ablation by bulky grain
Raw material are ground into nano particle (multi-layer nano particle), further by ultrasonic liquid-phase lift-off technology in a short time by nanometer
Particle removes the quantum dot into individual layer or few layer；The method of the present invention has used seldom chemical reagent, therefore the quantum dot generated
With higher purity and reduce chemical contamination.Compared with conventional method, method provided by the invention has operation letter
It is single, take short, the advantages of quantum dot purity is high.
Description of the drawings
Fig. 1 is that the transmission electron microscope image of boron nitride quantum dot prepared by the method for the present invention and high-resolution transmitted electron are shown
Micro- image.
Fig. 2-1 is the atomic force microscopy image of boron nitride quantum dot prepared by the method for the present invention.
Fig. 2-2 is the profile elevations h distribution of boron nitride quantum dot prepared by the method for the present invention.
Fig. 3 is the Raman spectrum that block hexagonal boron nitride and the method for the present invention prepare boron nitride quantum dot.
Fig. 4 is the photoluminescence spectra of boron nitride quantum dot prepared by the method for the present invention.
Fig. 5 is MoS2TEM (transmission electron microscope) result of quantum dot.
Fig. 6 is WS2TEM (transmission electron microscope) result of quantum dot.
Specific embodiment
With reference to specific embodiment, the present invention is described in further detail, it is described be explanation of the invention and
It is not to limit.
Embodiment 1
1) block BN materials are milled into small particle powder, 50mg powder is dispersed in 5mL N-Methyl pyrrolidones
(NMP) solution, and 300W power ultrasonic 2-3min are used, it is made to be uniformly dispersed.Sample after will be scattered takes out 300 μ L and relays
It puts in 40mL N-Methyl pyrrolidones (NMP) solution, and uses 300W power ultrasonic 2-3min, it is made to be uniformly dispersed, is obtained
Dispersion liquid.
2) 10mL is taken to be placed in 10mL beakers the dispersion liquid configured, is put into magnetic rotor, beaker is placed into magnetic
It on power blender, is stirred with the rotating speed of 400 turns/min, while power injects beaker for 400mW femtosecond lasers and carries out ablation.
3) after ablation 30min, liquid becomes faint yellow from pellucidity, and the sample that ablation synthesizes is centrifuged, and removes
Unreacted or the incomplete bulky grain of reaction, centrifugal acceleration are 10800 × g, and centrifugation time 10min is repeated twice.
4) supernatant after centrifugation is taken out, is placed in 50 milliliters of centrifuge tube and preserves.Merge four batches of supernatant (steps
40mL dispersion liquids are prepared in 1, are handled according to mono- batch of 10mL).
5) above-mentioned supernatant 20-30mL is taken to be put into progress ultrasonic liquid-phase stripping, ultrasound environments temperature in thermostatic ultrasonic pulverizer
Degree is arranged to 10 DEG C, ultrasonic power 600W, ultrasonic time 2h.
6) after ultrasonic liquid-phase is removed, sample taking-up is placed on shady and cool, ventilation and is preserved, obtains quantum dot solution.
Embodiment 2
1) by block MoS2Material is milled into small particle powder, and 50mg powder is dispersed in 5mL n,N-Dimethylformamide
(DMF) solution, and 350W power ultrasonic 2-3min are used, it is made to be uniformly dispersed.Sample after will be scattered takes out 300 μ L and relays
It puts in 40mL DMF solutions, and uses 300W power ultrasonic 2-3min, it is made to be uniformly dispersed, obtains dispersion liquid.
2) 10mL is taken to be placed in 10mL beakers the dispersion liquid configured, is put into magnetic rotor, beaker is placed into magnetic
It on power blender, is stirred with the rotating speed of 500 turns/min, while power injects beaker for 600mW femtosecond lasers and carries out ablation.
3) after ablation 90min, liquid becomes faint yellow from pellucidity, and the sample that ablation synthesizes is centrifuged, and removes
Unreacted or the incomplete bulky grain of reaction, centrifugal acceleration are 8000 × g, and centrifugation time 10min is repeated twice.
4) supernatant after centrifugation is taken out, is placed in 50 milliliters of centrifuge tube and preserves.Merge four batches of supernatant (steps
40mL dispersion liquids are prepared in 1).
5) above-mentioned supernatant is taken to be put into thermostatic ultrasonic pulverizer and carries out ultrasonic liquid-phase stripping, ultrasound environments temperature setting is
20 DEG C, ultrasonic power 700W, ultrasonic time 2.5h.
6) after ultrasonic liquid-phase is removed, sample taking-up is placed on shady and cool, ventilation and is preserved.
MoS2The results are shown in Figure 5 by the TEM of quantum dot.
Embodiment 3
1) by block WS2Material is milled into small particle powder, and 50mg powder is dispersed in 10mL n,N-Dimethylformamide
(DMF) solution, and 400W power ultrasonic 2-3min are used, it is made to be uniformly dispersed, obtains dispersion liquid.Sample after will be scattered takes out
200 μ L are reapposed in 40mL DMF solutions, and use 400W power ultrasonic 2-3min, it is made to be uniformly dispersed, is disperseed
Liquid.
2) 10mL is taken to be placed in 10mL beakers the dispersion liquid configured, is put into magnetic rotor, beaker is placed into magnetic
It on power blender, is stirred with the rotating speed of 400 turns/min, while power injects beaker for 500mW femtosecond lasers and carries out ablation.
3) after ablation 18min, liquid becomes faint yellow from pellucidity, and the sample that ablation synthesizes is centrifuged, and removes
Unreacted or the incomplete bulky grain of reaction, centrifugal acceleration are 12000 × g, and centrifugation time 12min is repeated twice.
4) supernatant after centrifugation is taken out, is placed in 50 milliliters of centrifuge tube and preserves.Merge four batches of supernatant (steps
40mL dispersion liquids are prepared in 1).
5) above-mentioned supernatant is taken to be put into thermostatic ultrasonic pulverizer and carries out ultrasonic liquid-phase stripping, ultrasound environments temperature setting is
15 DEG C, ultrasonic power 800W, ultrasonic time 2h.
6) after ultrasonic liquid-phase is removed, sample taking-up is placed on shady and cool, ventilation and is preserved.
WS2The results are shown in Figure 6 by the TEM of quantum dot.
Embodiment 4
1) by block MoSe2Material is milled into small particle powder, and 100mg powder is dispersed in 5mL N, N- dimethylacetamides
Amine (DMA) solution, and 500W power ultrasonic 2-3min are used, it is made to be uniformly dispersed, the sample after disperseing takes out 400 μ L again
It is placed in 40mL DMA solution, and uses 400W power ultrasonic 2-3min, it is made to be uniformly dispersed, obtains dispersion liquid.
2) 10mL is taken to be placed in 10mL beakers the dispersion liquid configured, is put into magnetic rotor, beaker is placed into magnetic
It on power blender, is stirred with the rotating speed of 300 turns/min, while power injects beaker for 200mW femtosecond lasers and carries out ablation.
3) after ablation 3h, liquid becomes faint yellow from pellucidity, and the sample that ablation synthesizes is centrifuged, and removal is not anti-
Should or it react incomplete bulky grain, centrifugal acceleration is 11000 × g, centrifugation time 8min, in triplicate.
4) supernatant after centrifugation is taken out, is placed in 10 milliliters of centrifuge tube and preserves.Merge four batches of supernatant (steps
40mL dispersion liquids are prepared in 1).
5) above-mentioned supernatant is taken to be put into thermostatic ultrasonic pulverizer and carries out ultrasonic liquid-phase stripping, ultrasound environments temperature setting is
5 DEG C, ultrasonic power 800W, ultrasonic time 1.5h.
6) after ultrasonic liquid-phase is removed, sample taking-up is placed on shady and cool, ventilation and is preserved.
Embodiment 5
1) by block WSe2Material is milled into small particle powder, and 50mg powder is dispersed in 10mL dimethyl sulfoxide (DMSO)s (DMSO)
Solution, and 600W power ultrasonic 2-3min are used, it is made to be uniformly dispersed, the sample after disperseing takes out 1000 μ L and is reapposed over
In 40mL DMA solution, and 400W power ultrasonic 2-3min are used, it is made to be uniformly dispersed, obtains dispersion liquid.
2) 10mL is taken to be placed in 10mL beakers the dispersion liquid configured, is put into magnetic rotor, beaker is placed into magnetic
It on power blender, is stirred with the rotating speed of 500 turns/min, while power injects beaker for 600mW femtosecond lasers and carries out ablation.
3) after ablation 80min, liquid becomes faint yellow from pellucidity, and the sample that ablation synthesizes is centrifuged, and removes
Unreacted or the incomplete bulky grain of reaction, centrifugal acceleration are 9000 × g, centrifugation time 10min, are repeated secondary.
4) supernatant after centrifugation is taken out, is placed in 50 milliliters of centrifuge tube and preserves.Merge four batches of supernatant (steps
40mL dispersion liquids are prepared in 1).
5) above-mentioned supernatant is taken to be put into thermostatic ultrasonic pulverizer and carries out ultrasonic liquid-phase stripping, ultrasound environments temperature setting is
10 DEG C, ultrasonic power 800W, ultrasonic time 1.5h.
6) after ultrasonic liquid-phase is removed, sample taking-up is placed on shady and cool, ventilation and is preserved.
Embodiment 6
Tem study (the results are shown in Figure 1), original are carried out to the boron nitride quantum dot synthesized by embodiment 1
Sub- force microscope analyzes (result is as shown in Fig. 2-1 and Fig. 2-2), Raman spectrum analysis (the results are shown in Figure 3) and detects its light
Photoluminescence spectrum (the results are shown in Figure 4).
As shown in Figure 1, transmission electron microscope image shows that the quantum dot of synthesis is evenly distributed, no any cluster generates, high
Resolution Transmission Electron micro-image shows the spacing of lattice 0.22cm of quantum dot, it is known that corresponding boron nitride (100) crystal face illustrates to close
Into quantum dot be boron nitride.
As shown in Fig. 2-1 and Fig. 2-2, quantum dot atomic force microscopy image and its profile elevations h illustrate the boron nitride amount synthesized
The height of son point is about 1-2nm, and quantum dot is individual layer or few layer structure.
Illustrate the Raman spectrum of hexagonal boron nitride (h BN Powder) and boron nitride quantum dot (BNQDs) in Fig. 3, two
Kind material is in 1376cm-1Place there are an apparent Raman peaks, shows still to protect using the boron nitride quantum dot that the present invention synthesizes
The structure of B-N is hold, which does not construct boron nitride in itself damages.
Fig. 4 gives the photoluminescence spectra of boron nitride quantum dot, it is observed that having in 400nm-500nm wave bands bright
Aobvious fluorescence emission peak, it was demonstrated that the nano material of the method for the present invention synthesis has stronger fluorescent characteristic, can be used as bio-imaging
With the fluorescence probe of bio-sensing.
The present invention proposes a kind of preparation method of quantum dot, is removed including femtosecond laser liquid phase ablation technology and ultrasonic liquid-phase
Two parts of technology.The two-dimensional material of bulk multilayer is crushed the nanometer for multilayer by femtosecond laser liquid phase ablation technology first
Then the nano particle of multilayer is removed the quantum dot into individual layer by grain using ultrasonic liquid-phase lift-off technology.And others add at present
Work method is first to remove bulk multilayer two-dimension material into individual layer sheet, then is aided with other means and crushes sheet for quantum dot.
The advantages of present invention has compared with other methods and saves the time, easy to operate, raising efficiency, while because the invention is not drawn
Enter chemical means, therefore the quantum dot purity synthesized is high.The present invention introduces new thinking for synthesizing new nano material, and is
It synthesizes regulatable quantum dot and provides possibility.
Claims (9)
1. a kind of preparation method of quantum dot solution, the quantum dot is boron nitride quantum dot or transient metal sulfide quantum
Point, which is characterized in that including step：
1) boron nitride powder or transient metal sulfide powder are dispersed in organic inert solvent, and disperseed under ultrasound
It is even, obtain dispersion liquid；
2) ablation is carried out in the femtosecond laser for being under stiring, 200mW~600mW with power injection dispersion liquid, obtains ablation liquid；
3) ablation liquid obtains supernatant by centrifuging；
4) gained supernatant is subjected to ultrasonic liquid-phase stripping, obtains quantum dot solution.
2. the preparation method of quantum dot solution as described in claim 1, which is characterized in that described organic lazy in step 1)
Property solvent for N-Methyl pyrrolidone, N,N-dimethylformamide, DMAC N,N' dimethyl acetamide, one kind in dimethyl sulfoxide (DMSO) or
It is a variety of.
3. the preparation method of quantum dot solution as described in claim 1, which is characterized in that in step 1), in dispersion liquid, nitrogen
The concentration for changing boron powder or transient metal sulfide powder is 50~200mg/L.
4. the preparation method of quantum dot solution as described in claim 1, which is characterized in that in step 2), femtosecond laser note
The gross energy entered：Quality=200 of boron nitride powder or transient metal sulfide powder~1200Wh/g, wherein, femtosecond swashs
The gross energy of light injection is the power of femtosecond laser and the product of ablation time.
5. the preparation method of quantum dot solution as described in claim 1, which is characterized in that in step 2), the speed of stirring
For 300~500 turns/min.
6. the preparation method of quantum dot solution as described in claim 1, which is characterized in that in step 3), centrifuge every time
Time is 8~12min.
7. the preparation method of quantum dot solution as described in claim 1, which is characterized in that in step 3), centrifugal rotational speed is
8000~12000 × g.
8. the preparation method of quantum dot solution as described in claim 1, which is characterized in that in step 3), ablation liquid repeats 2
~3 operations for centrifuging and retaining supernatant, obtain supernatant.
9. the preparation method of quantum dot solution as described in claim 1, which is characterized in that in step 4), ultrasonic liquid-phase stripping
From condition be：Ultrasound environments temperature is 5~20 DEG C, and ultrasonic power is 400~800w.
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| CN109399724A (en) * | 2018-11-26 | 2019-03-01 | 深圳大学 | The preparation method of rhenium disulfide quantum dot |
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Cited By (10)
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| CN108906013A (en) * | 2018-07-23 | 2018-11-30 | 合肥工业大学 | A kind of method that ultrasonication prepares titanium dioxide quantum dot |
| CN108906013B (en) * | 2018-07-23 | 2021-09-14 | 合肥工业大学 | Method for preparing titanium dioxide quantum dots through ultrasonic crushing |
| CN109317183A (en) * | 2018-11-12 | 2019-02-12 | 湖南大学 | A kind of boron nitride quantum dot/ultra-thin porous carbonitride composite photocatalyst material and its preparation method and application |
| 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 |
| CN110092359A (en) * | 2019-05-27 | 2019-08-06 | 华东师范大学 | A kind of method of liquid phase removing two selenizing vanadium quantum dots of preparation |
| CN110272048A (en) * | 2019-06-17 | 2019-09-24 | 西安电子科技大学 | A kind of preparation method of two-dimensional layer nano material MXene quantum dot |
| CN110194464A (en) * | 2019-06-25 | 2019-09-03 | 中北大学 | A kind of preparation method and application of boron quantum dot |
| CN110194464B (en) * | 2019-06-25 | 2022-06-07 | 中北大学 | Preparation method and application of boron quantum dots |
| CN113697822A (en) * | 2020-05-20 | 2021-11-26 | 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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| CN108046223B (en) | 2020-10-27 |
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