CN106190120A - A kind of black phosphorus quantum dot and preparation method thereof - Google Patents
A kind of black phosphorus quantum dot and preparation method thereof Download PDFInfo
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Abstract
The invention provides the preparation method of a kind of black phosphorus quantum dot, including: the black phosphorus that particle diameter is 5～50 μm under anaerobic, is dispersed in the first organic solvent by (1), obtains the first dispersion liquid that black phosphorus concentration is 0.6～1.2mg/mL；(2) using described first organic solvent that described first dispersion liquid is diluted 5～10 times, add sodium hydroxide, obtain the second dispersion liquid, in described second dispersion liquid, black phosphorus is 0.006～0.012:1 with the mass ratio of sodium hydroxide；(3) described second dispersion liquid is placed in hermetic container, reacting by heating 6～18h at temperature is 120～160 DEG C, gained reactant liquor is cooled to room temperature, centrifugal, collect supernatant, obtain black phosphorus quantum dot.The method technique is simple to operation, and productivity is higher, favorable reproducibility, and the black phosphorus sheet layer material size that obtains in prior art can be overcome compared with the defect such as big, productivity is relatively low.Present invention also offers a kind of black phosphorus quantum dot.
Description
Technical field
The present invention relates to novel nano-material field, particularly relate to a kind of black phosphorus quantum dot and preparation method thereof.
Background technology
As a kind of allotrope of phosphorus, New Two Dimensional stratified material black phosphorus, have similar but be different from Graphene
The natural pleated structure of lamellar structure, the pleated structure of this uniqueness result in black phosphorus and has many unique physical propertys, as
Black phosphorus possesses the unexistent semiconductor gap of Graphene and is direct band gap, i.e. electronic conduction can carry (conduction band) bottom with non-conductive
(valence band) top can be carried at same position, it is achieved from non-conductive conduction, electronic values needs absorbability, it means that black phosphorus can
As variable semiconductor, can be with direct-coupling with light, spectrum includes whole visible ray near infrared region.Therefore, black phosphorus exists
The field such as nano optoelectronics, biomedicine has broad application prospects, such as: photoelectric device, sensor, switch etc..And it is black
Phosphorus quantum dot is because it has extra small size and has more application prospect at the aspect such as optical markings, treatment of cancer, therefore, and black phosphorus
Quantum dot prepare great realistic meaning.
At present, being by mechanically pulling off the technology such as method (as adhesive tape tears point-score), chemical vapour deposition technique, scholars are
Prepare the black phosphorus material of lamellar.But, the productivity of lamellar black phosphorus prepared by mechanical stripping method is relatively low, is not suitable for for manufacturer
Industry application material, and complex operation, scantling time-consuming long, that obtain are relatively big, how at micron order；And chemical vapour deposition technique
The amount of the black phosphorus sheet of preparation is considerably less, and is difficult to repeat.Therefore, it is badly in need of developing a kind of extensive preparation small size black phosphorus quantum
The convenient method of point.
Summary of the invention
In view of this, the invention provides a kind of black phosphorus quantum dot and preparation method thereof, this preparation method will be by grinding
After block black phosphorus disperse in organic solvent, be placed in the hermetic container under high temperature heat certain time, it is possible to obtain point
Scattered property is preferable, the black phosphorus quantum dot of size uniformity, and the size of obtained black phosphorus quantum dot is less, about 1～5nm, and at purple
Outer visible region presents obvious absorption characteristic.The method technique is simple to operation, and productivity is higher, favorable reproducibility, and
Can realize preparing on a large scale, environment is not produced secondary pollution problem.
First aspect, the invention provides the preparation method of a kind of black phosphorus quantum dot, comprises the following steps:
(1) under anaerobic, the black phosphorus that particle diameter is 5～50 μm is dispersed in the first organic solvent, obtains first point
Dissipating liquid, in described first dispersion liquid, the concentration of black phosphorus is 0.6～1.2mg/mL；
(2) use described first organic solvent that described first dispersion liquid is diluted 5～10 times, add sodium hydroxide afterwards,
Obtaining the second dispersion liquid, in described second dispersion liquid, black phosphorus is 0.006～0.012:1 with the mass ratio of sodium hydroxide；
(3) described second dispersion liquid is placed in hermetic container, reacting by heating 6～18h at temperature is 120～160 DEG C,
After completion of the reaction, gained reactant liquor is cooled to room temperature, centrifugal, collect supernatant, obtain black phosphorus quantum dot.
Preferably, in described second dispersion liquid, the concentration of black phosphorus is 0.06～0.12mg/mL.
In step (2), the second dispersion liquid there was added sodium hydroxide, on the one hand the sodium ion in sodium hydroxide and hydroxyl
Ion can be intercalation in black phosphorus lamella, weakens the Van der Waals force between black phosphorus lamella, improves charge stripping efficiency, the most
Remaining hydroxide ion can adsorb the effect playing protection black phosphorus on black phosphorus surface, improves the stability of black phosphorus.Therefore, originally
Preferably making the mass ratio of the quality of black phosphorus and described sodium hydroxide in the second dispersion liquid in application is 0.006～0.012:1.
If it addition, naoh concentration is the lowest, then the probability during it is intercalation into black phosphorus lamella will reduce, so in order to
Reaching preferably peeling effect, the general sodium hydroxide added can excess.If but if adding too many NaOH, because of hydroxide
Sodium dissolubility in the second dispersion liquid is not the highest, adds and can relatively waste material too much.
Preferably, in step (2), take described first dispersion liquid 2～4mL, add 18～36mL described first organic
Solvent, adds the sodium hydroxide of 200～400mg afterwards, obtains the second dispersion liquid.
In the application, in step (2), at temperature is 120～160 DEG C, heating 6～18h is to carry out the stripping of black phosphorus, high
The energy that temperature provides can weaken the Van der Waals force between black phosphorus lamella so that it is is more easily peelable.
Preferably, in step (2), described hermetic container is autoclave (such as politef reactor) or three mouthfuls
Bottle.
Preferably, when described hermetic container is there-necked flask, also it is stirred during described reacting by heating, its
In, the speed of described stirring is 3000-4000 rev/min.
Preferably, the size of described black phosphorus quantum dot is 1～5nm.The most excellent for 2-4nm.
Preferably, in step (1), described particle diameter be the black phosphorus of 5～50 μm be by being ground obtaining by black phosphorus block.
It is further preferred that the grinding of described black phosphorus block is carried out (under oxygen-free environment) under vacuum conditions.Preferably
Carry out in having the glove box of protection of nitrogen, and in process of lapping, add some first organic solvents.
It is highly preferred that described black phosphorus block is to utilize white phosphorus to convert under High Voltage and high-temperature and formed.
Preferably, described first organic solvent includes N-Methyl pyrrolidone (NMP), dimethylformamide (DMF), diformazan
One or more in base sulfoxide (DMSO), methylimidazole quinoline (DMEU), acetone and dehydrated alcohol.
It is highly preferred that described first organic solvent is N-Methyl pyrrolidone.
Preferably, the temperature of described reacting by heating is 120～135 DEG C.
It is further preferred that the temperature of described reacting by heating is 120～130 DEG C.
Preferably, the temperature of described reacting by heating is 135～160 DEG C.
It is further preferred that the temperature of described reacting by heating is 140～160 DEG C.
Preferably, in step (2), the time of described reacting by heating is 6～12h.
It is further preferred that the time of described reacting by heating is 8～12h.
Preferably, the time of described reacting by heating is 14～18h.
It is further preferred that the time of described reacting by heating is 16～18h.
In the embodiment of the present invention, the temperature of described reacting by heating is 120 DEG C, 125 DEG C, 130 DEG C, 135 DEG C, 140 DEG C, 150
℃、160℃.The time of described reacting by heating can be 6h, 8h, 10h, 12h, 14h, 16h, 18h.
Preferably, in step (3), described centrifugal rotating speed is 6000～9000 revs/min, and centrifugation time is that 10-30 divides
Clock.It is preferably 15-25 minute.
Preferably, in step (3), described being centrifuged is to carry out under nitrogen protection in glove box.
Preferably, described step (3) also includes:
After described collection supernatant, described supernatant is carried out high speed centrifugation 10-30min, collect solid product or
Described solid product is distributed in the second organic solvent, obtains black phosphorus quantum dot.
Preferably, described ultracentrifugal rotating speed is 10000-12000rpm.
Preferably, described second organic solvent include N-Methyl pyrrolidone (NMP), dimethylformamide (DMF),
One or more in dimethyl sulfoxide (DMSO), methylimidazole quinoline (DMEU), acetone and dehydrated alcohol.
Described first organic solvent and described second organic solvent, can be homogeneous solvent, it is also possible to for not homogeneous solvent.
The preparation method of the black phosphorus quantum dot that first aspect present invention provides, to realize the stripping to black phosphorus block, this side
Method technique is simple to operation, can carry out mass stripping, peels off productivity higher, compares current mechanical stripping method and chemistry gas
Phase sedimentation etc. has obvious advantage, can obtain that the controlled monodispersity of size is good, the small size black phosphorus quantum dot of size uniformity,
Easily realize low cost industrialization to produce.
Preparation method based on first aspect present invention, it is possible to achieve from the extensive product of black phosphorus solid to black phosphorus quantum dot
Prepared by industry, lay the foundation in the application of biomedical sector, optoelectronic areas for black phosphorus quantum dot.
Second aspect, present invention also offers the black phosphorus quantum dot prepared by above-mentioned preparation method.Described black phosphorus amount
The size of son point is 1～5nm.
The particle diameter narrow distribution of obtained black phosphorus quantum dot, size is less, shows substantially in ultraviolet-visible light region
Absorption characteristic, can apply to prepare the biomedical frontier fields such as photo-thermal therapy medicine, optical markings medicine, sensor.
The advantage of the embodiment of the present invention will partly illustrate, a part according to description be aobvious and
It is clear to, or can be known by the enforcement of the embodiment of the present invention.
Accompanying drawing explanation
Fig. 1 be the black phosphorus quantum dot for preparing of the embodiment of the present invention 1 ultraviolet-visible in N-Methyl pyrrolidone solution-
Near-infrared absorption spectrum figure；
Fig. 2 is the low power transmission electron microscope picture (TEM) of the black phosphorus quantum dot that the embodiment of the present invention 1 prepares；
Fig. 3 is high-resolution-ration transmission electric-lens (HRTEM) figure of the black phosphorus quantum dot that the embodiment of the present invention 1 prepares；
Fig. 4 is the Raman spectrogram of the black phosphorus quantum dot that the embodiment of the present invention 1 prepares；
Fig. 5 be the black phosphorus quantum dot for preparing of the embodiment of the present invention 4 ultraviolet-visible in N-Methyl pyrrolidone solution-
Near-infrared absorption spectrum figure；
Fig. 6 is the low power transmission electron microscope picture of the black phosphorus quantum dot that the embodiment of the present invention 4 prepares.
Detailed description of the invention
The following stated is the preferred implementation of the embodiment of the present invention, it is noted that for the common skill of the art
For art personnel, on the premise of without departing from embodiment of the present invention principle, it is also possible to make some improvements and modifications, these improve
With the protection domain that retouching is also considered as the embodiment of the present invention.
Divide multiple embodiment that the embodiment of the present invention is further detailed below.The embodiment of the present invention be not limited to
Under specific embodiment.In the range of constant principal right, carrying out change that can be suitable is implemented.
In the embodiment of the present invention, described black phosphorus block is to buy from Smart-Elements company.
Embodiment 1
The preparation method of a kind of black phosphorus quantum dot, comprises the steps:
(1) in the glove box of inflated with nitrogen, weigh the block black phosphorus of 10mg, ground and be distributed to the N-methyl of 10mL
In ketopyrrolidine, seal, obtain first dispersion liquid of 1mg/mL；
(2) taking above-mentioned first dispersion liquid 2mL, the N-Methyl pyrrolidone adding 18mL is diluted, and is subsequently adding 200mg
Sodium hydroxide, be uniformly mixing to obtain the second dispersion liquid；
(3) joining in politef autoclave by above-mentioned second dispersion liquid, in temperature is 140 DEG C, heating is anti-
Answer 18h, after gained reactant liquor is cooled to room temperature, be centrifuged 20 minutes under the rotating speed of 7000 revs/min, collect supernatant,
To the black phosphorus quantum dot being dispersed in N-Methyl pyrrolidone.
The present embodiment 1 gained black phosphorus quantum dot is more stable, can at room temperature deposit 1 month.By black for the present embodiment 1 gained
Phosphorus quantum dot characterizes, and as shown in Figure 1 to 4, wherein, Fig. 1 is that black phosphorus quantum dot is at N-Methyl pyrrolidone solution to result
In UV-visible-near infrared absorption figure；Fig. 2 is the low power transmission electron microscope picture of black phosphorus quantum dot；Fig. 3 is black phosphorus quantum
The high-resolution-ration transmission electric-lens figure of point；Fig. 4 is the Raman spectrogram of black phosphorus quantum dot.
As can be seen from Figure 1: black phosphorus quantum dot shows obvious absorption characteristic in 300-900nm region, it absorbs
Peak value is about at 500nm, and when this is less with the size of black phosphorus quantum dot, its band gap increased relation；Fig. 2 can be seen that institute
The monodispersity of the black phosphorus quantum dot prepared is good, size uniformity, and its size is at about 3nm；Can significantly see black from Fig. 3
The lattice fringe of phosphorus quantum dot atomic layer, wherein, spacing of lattice is (014) crystal face that 0.21nm corresponds to black phosphorus crystal；From Fig. 4
In can be seen that the Raman spectrogram of black phosphorus quantum dot has obvious blue shift (moving right) relative to block black phosphorus, it was demonstrated that black
Phosphorus quantum dot ratio is relatively thin.
Embodiment 2
The preparation method of a kind of black phosphorus quantum dot, comprises the steps:
In the glove box of inflated with nitrogen, weigh the block black phosphorus of 30mg, ground and be distributed to the N-methylpyrrole of 25mL
In alkanone, seal, obtain first dispersion liquid of 1.2mg/mL；
Take above-mentioned first dispersion liquid 4mL, add the N-Methyl pyrrolidone of 36mL, it is possible to additionally incorporate the sodium hydroxide of 400mg,
It is uniformly mixing to obtain the second dispersion liquid；
Above-mentioned second dispersion liquid is joined in autoclave, reacting by heating 14h in temperature is 120 DEG C, has heated
Finish, after system is cooled to room temperature, to gained reactant liquor under the rotating speed of 9000 revs/min centrifugal 10 minutes, collect supernatant；
Again the supernatant collected being carried out high speed centrifugation 20min, rotating speed is 12000rpm, collects solid product or by described solid product
It is distributed in dehydrated alcohol, obtains being dispersed in dehydrated alcohol, the black phosphorus quantum dot of a size of 4nm.
Embodiment 3
The preparation method of a kind of black phosphorus quantum dot, comprises the steps:
In the glove box of inflated with nitrogen, weigh the block black phosphorus of 12mg, ground and be distributed to the N-methylpyrrole of 20mL
In alkanone, seal, obtain first dispersion liquid of 0.6mg/mL；
Take above-mentioned first dispersion liquid 3mL, add the dimethylformamide of 27mL, it is possible to additionally incorporate the sodium hydroxide of 300mg, stir
Mix and uniformly obtain the second dispersion liquid；
Above-mentioned second dispersion liquid is joined in autoclave, reacting by heating 10h in temperature is 130 DEG C, has heated
Finish, after system is cooled to room temperature, to gained reactant liquor under the rotating speed of 6000 revs/min centrifugal 30 minutes, collect supernatant,
Obtain the black phosphorus quantum dot being dispersed in N-Methyl pyrrolidone.
Embodiment 4
The preparation method of a kind of black phosphorus quantum dot, comprises the steps:
In the glove box of inflated with nitrogen, weigh the block black phosphorus of 25mg, ground and be distributed to the N-methylpyrrole of 25mL
In alkanone, seal, obtain first dispersion liquid of 1mg/mL；
Take above-mentioned first dispersion liquid 2mL, add the N-Methyl pyrrolidone of 18mL, it is possible to additionally incorporate the sodium hydroxide of 200mg,
It is uniformly mixing to obtain the second dispersion liquid；
Above-mentioned second dispersion liquid is joined in there-necked flask, heated and stirred 6h at temperature is 140 DEG C, wherein stirs
Speed is 4000 revs/min；After system is cooled to room temperature, gained reactant liquor is centrifuged 20 points under the rotating speed of 7000 revs/min
Clock, collects supernatant, obtains the black phosphorus quantum dot being dispersed in N-Methyl pyrrolidone.
Being characterized by the black phosphorus quantum dot of the present embodiment 4 gained, as shown in figures 5 and 6, wherein, Fig. 5 is black phosphorus to result
Quantum dot UV-visible-near infrared absorption figure in N-Methyl pyrrolidone solution；Fig. 6 is that the embodiment of the present invention 4 is made
The low power transmission electron microscope picture of the black phosphorus quantum dot obtained.
As can be seen from Figure 5: black phosphorus quantum dot shows obvious absorption characteristic in 300-900nm region, from Fig. 6
Can be seen that the size uniformity of black phosphorus quantum dot, good dispersion, its size is at about 2.6nm.
Additionally, with under equal conditions, the black phosphorus quantum dot (3nm) using autoclave to prepare is compared, and the present embodiment 4 is made
The particle diameter of the black phosphorus quantum dot obtained is smaller, and this is probably and also uses external force stirring caused.
Embodiment 5
In the glove box of inflated with nitrogen, weigh the block black phosphorus of 30mg, ground and be distributed to the N-methylpyrrole of 15mL
In alkanone, seal, obtain first dispersion liquid of 1.2mg/mL；
Take above-mentioned first dispersion liquid 3mL, add the N-Methyl pyrrolidone of 27mL, it is possible to additionally incorporate the sodium hydroxide of 300mg,
It is uniformly mixing to obtain the second dispersion liquid；
Above-mentioned second dispersion liquid is joined in there-necked flask, heated and stirred 10h at temperature is 120 DEG C, wherein stirs
Speed be 3500 revs/min；After question response system is cooled to room temperature, to gained reactant liquor under the rotating speed of 6000 revs/min from
The heart 25 minutes, collects supernatant, obtains the black phosphorus quantum dot being dispersed in N-Methyl pyrrolidone.
Embodiment 6
In the glove box of inflated with nitrogen, weigh the block black phosphorus of 12mg, ground and be distributed to the N-methylpyrrole of 20mL
In alkanone, seal, obtain first dispersion liquid of 0.6mg/mL；
Take above-mentioned first dispersion liquid 4mL, add the N-Methyl pyrrolidone of 36mL, it is possible to additionally incorporate the sodium hydroxide of 400mg,
It is uniformly mixing to obtain the second dispersion liquid；
Above-mentioned second dispersion liquid is joined in there-necked flask, heated and stirred 8h at temperature is 160 DEG C, wherein stirs
Speed is 3000 revs/min；Then after reaction system being cooled to room temperature, to gained reactant liquor under 9000 revs/min of rotating speeds from
The heart 15 minutes, takes supernatant, obtains being dispersed in N-Methyl pyrrolidone, the black phosphorus quantum dot of a size of 3.5nm.
The foregoing is only presently preferred embodiments of the present invention, not in order to limit the present invention, all essences in the present invention
Any amendment, equivalent and the improvement etc. made within god and principle, should be included within the scope of the present invention.
Claims (10)
1. the preparation method of a black phosphorus quantum dot, it is characterised in that comprise the following steps:
(1) under anaerobic, the black phosphorus that particle diameter is 5～50 μm is dispersed in the first organic solvent, obtains the first dispersion liquid,
In described first dispersion liquid, the concentration of black phosphorus is 0.6～1.2mg/mL；
(2) use described first organic solvent that described first dispersion liquid is diluted 5～10 times, add sodium hydroxide afterwards, obtain
Second dispersion liquid, in described second dispersion liquid, black phosphorus is 0.006～0.012:1 with the mass ratio of sodium hydroxide；
(3) described second dispersion liquid is placed in hermetic container, reacting by heating 6～18h at temperature is 120～160 DEG C, reaction
After, gained reactant liquor is cooled to room temperature, centrifugal, collect supernatant, obtain black phosphorus quantum dot.
2. preparation method as claimed in claim 1, it is characterised in that in step (2), described hermetic container is autoclave
Or there-necked flask.
3. preparation method as claimed in claim 2, it is characterised in that when described hermetic container is there-necked flask, add described
Being stirred during heat, wherein, the speed of described stirring is 3000-4000 rev/min.
4. preparation method as claimed in claim 1, it is characterised in that the size of described black phosphorus quantum dot is 1～5nm.
5. preparation method as claimed in claim 1, it is characterised in that in described second dispersion liquid the concentration of black phosphorus be 0.06～
0.12mg/mL。
6. preparation method as claimed in claim 1, it is characterised in that the temperature of described reacting by heating is 140～160 DEG C, institute
The time stating reacting by heating is 14～18 hours.
7. preparation method as claimed in claim 1, it is characterised in that described first organic solvent be N-Methyl pyrrolidone,
One or more in dimethylformamide, dimethyl sulfoxide, methylimidazole quinoline, acetone and dehydrated alcohol.
8. preparation method as claimed in claim 1, it is characterised in that described particle diameter be the black phosphorus of 5～50 μm be by by black
Phosphorus block is ground obtaining.
9. preparation method as claimed in claim 1, it is characterised in that described centrifugal rotating speed is 6000～9000 revs/min,
Centrifugation time is 10～30 minutes.
10. a black phosphorus quantum dot, it is characterised in that use the method described in any one of claim 1～9 to prepare is described black
The size of phosphorus quantum dot is 1～5nm.
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