CN104211050A - Preparation method of suspension liquid and powder of graphene quantum dot - Google Patents
Preparation method of suspension liquid and powder of graphene quantum dot Download PDFInfo
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- CN104211050A CN104211050A CN201410336362.8A CN201410336362A CN104211050A CN 104211050 A CN104211050 A CN 104211050A CN 201410336362 A CN201410336362 A CN 201410336362A CN 104211050 A CN104211050 A CN 104211050A
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Abstract
The invention discloses a preparation method of a suspension liquid and a powder of graphene quantum dots. The method includes following steps: preparing the suspension liquid of the graphene quantum dots in one step from fullerene in a manner of chemical oxidation cleavage, removing impurity ions from the suspension liquid, and then performing a drying process to obtain the powder of the graphene quantum dots. In the invention, problems of complex technology and high cost in preparation of the suspension liquid and the powder of the graphene quantum dots are solved. The preparation method is simple in operation, can quickly prepare the suspension liquid and the powder of the graphene quantum dots in macro scale in an amplifying manner and is high in yield. The graphene quantum dots are uniform in size distribution and are excellent in water solubility.
Description
Technical field
The invention belongs to photoelectric technology, biomarker field, particularly, relate to a kind of preparation method of quantum dot, relate more specifically to the large batch of preparation method of a kind of graphene quantum dot suspension and powder.
Background technology
Graphene, due to its excellent electricity, calorifics, mechanics, optical characteristics, since it is found 2004, has just been subject to extensive concern.But Graphene is zero band gap material, which has limited its application at semiconducter device and field of photoelectric devices.Graphene quantum dot, by size is reduced to nanoscale, utilizes quantum local effect to open band gap, thus makes the transition of electronics and compound become possibility, has expanded the application of Graphene in photoelectric field and biomarker field.
The existing method preparing graphene quantum dot is generally from presomas such as graphene oxide, Graphene, carbon nanotubes, by the effect of acid with strong oxidizing property, is cut to nano-scale.By high speed centrifugation, large size removing just to can be obtained the quantum dot of nano-scale in the process of preparation, such preparation process causes the productive rate of quantum dot very low, be usually less than 10%, thus cause the expensive of graphene quantum dot, and obtained quantum dot size distributes very heterogeneity.
Summary of the invention
The object of the invention is, for prior art above shortcomings part, to provide a kind of preparation method preparing graphene quantum dot suspension and powder in enormous quantities, the technical problem that solve is the productive rate promoting graphene quantum dot, thus reduces costs.
Above-mentioned purpose of the present invention is that the technical scheme can crossed below is realized:
A preparation method for graphene quantum dot suspension and powder, from soccerballene, makes graphene quantum dot suspension with chemical oxidation cutting, then removes the foreign ion in suspension, obtain graphene quantum dot powder finally by drying.
As described in a kind of graphene quantum dot suspension and the preparation method of powder, wherein said chemical oxidation cutting soccerballene presoma soccerballene and the vitriol oil is mixed in ice-water bath and stirs simultaneously, the consumption of soccerballene and the vitriol oil is the 0.5g soccerballene proportioning vitriol oil 10 ~ 100ml, stirring velocity 100 ~ 1000rpm; Then slowly add SODIUMNITRATE, potassium permanganate, the consumption of SODIUMNITRATE is 0 ~ 3 times of soccerballene quality used, and the consumption of potassium permanganate is 1 ~ 6 times of soccerballene quality used; After potassium permanganate has added, ice-water bath 0 ~ 90min, then changes ice-water bath into water bath with thermostatic control, and temperature is 20 ~ 40 DEG C, insulation 10min ~ 24h; Then add pure water, pure water used be aforementioned soccerballene, the vitriol oil, SODIUMNITRATE, 2 ~ 5 times of potassium permanganate mixeding liquid volume; Bath temperature is warming up to 70 ~ 100 DEG C, insulation 0 ~ 90min.
As described in a kind of graphene quantum dot suspension and the preparation method of powder, foreign ion in wherein said removal suspension is that the graphene quantum dot suspension filtered made from chemical oxidation cutting is removed macrobead, the aperture of filter membrane used is 0.01 ~ 0.22um, then dialyse in dialysis tubing, change water every day three times, the molecular weight cut-off of dialysis tubing used is 500 ~ 14000, obtains graphene quantum dot suspension.
As described in a kind of graphene quantum dot suspension and the preparation method of powder, wherein said drying be by the suspension Air drying obtained after the foreign ion eliminated in suspension or in baking oven, electric furnace, freeze drier drying obtain graphene quantum dot powder.
According to the preparation method of described a kind of graphene quantum dot suspension and powder, wherein said presoma soccerballene is one or more in C20, C36, C44, C50, C60, C70, C76, C80, C84, C90, C94, C120, C180, C540, and described vitriol oil massfraction is 98%.
More specifically, the present invention is by the following technical solutions: one, chemical oxidation cutting soccerballene: presoma soccerballene and the vitriol oil are mixed in ice-water bath and also stir simultaneously, soccerballene used comprises C20, C36, C44, C50, C60, C70, C76, C80, C84, C90, C94, C120, C180, C540 etc., vitriol oil massfraction used is 98%, consumption is the 0.5 gram of soccerballene proportioning vitriol oil 10 ~ 100ml, and stirring velocity is at 100 ~ 1000rpm; Then slowly add in SODIUMNITRATE, potassium permanganate one or more, the consumption of SODIUMNITRATE is 0 ~ 3 times of soccerballene quality used, and the consumption of potassium permanganate is 1 ~ 6 times of soccerballene quality used; Potassium permanganate adds completely, and the ice-water bath time is 0 ~ 90min, then changes ice-water bath into water bath with thermostatic control, and temperature is a temperature between 20 ~ 40 degree, and soaking time is 10min ~ 24h; Then add pure water, pure water used be aforementioned soccerballene, the vitriol oil, SODIUMNITRATE, 2 ~ 5 times of potassium permanganate mixeding liquid volume; Bath temperature is warming up to a temperature between 70 ~ 100 degree, insulation 0 ~ 90min.Two, foreign ion is removed: the suspension filtered finally obtained in the first step is removed macrobead, and the aperture of filter membrane used is 0.01 ~ 0.22um; Then dialyse in dialysis tubing, change water every day three times, the molecular weight cut-off of dialysis tubing used is 500 ~ 14000, and dialysis time 3 ~ 7 days, obtains graphene quantum dot suspension.Three, dry: by the suspension Air drying finally obtained in second step or in baking oven, electric furnace, freeze drier drying obtain graphene quantum dot powder.
Presoma of the present invention is soccerballene, comprises one or more in C20, C36, C44, C50, C60, C70, C76, C80, C84, C90, C94, C120, C180, C540 etc.
Chemical oxidation cutting soccerballene of the present invention obtains graphene quantum dot, by the successively mixing in ice-water bath of one or more in soccerballene, the vitriol oil and saltpetre, potassium permanganate, the consumption of the vitriol oil is the vitriol oil of 0.5g soccerballene proportioning 10 ~ 100ml massfraction 98%, potassium permanganate consumption is 1 ~ 6 times of soccerballene quality used, mixing process is carried out in ice-water bath and with stirring, stirring velocity is 100 ~ 1000rpm.
Chemical oxidation cutting soccerballene of the present invention obtains graphene quantum dot, that the consumption of the vitriol oil is the vitriol oil of 0.5g soccerballene proportioning 10 ~ 100ml massfraction 98% by the successively mixing in ice-water bath of one or more in soccerballene, the vitriol oil and saltpetre, potassium permanganate.
Chemical oxidation cutting soccerballene of the present invention obtains graphene quantum dot, is that the consumption of SODIUMNITRATE is 0 ~ 3 times of soccerballene quality used by the successively mixing in ice-water bath of one or more in soccerballene, the vitriol oil and saltpetre, potassium permanganate.
Chemical oxidation cutting soccerballene of the present invention obtains graphene quantum dot, is that potassium permanganate consumption is 1 ~ 6 times of soccerballene quality used by the successively mixing in ice-water bath of one or more in soccerballene, the vitriol oil and saltpetre, potassium permanganate.
Chemical oxidation cutting soccerballene of the present invention obtains graphene quantum dot, by one or more in soccerballene, the vitriol oil and saltpetre, potassium permanganate successively mixing, mixing is carried out in ice-water bath, and after potassium permanganate has added, the ice-water bath time is 0 ~ 90min.
Chemical oxidation cutting soccerballene of the present invention obtains graphene quantum dot, one or more mixed solution in soccerballene, the vitriol oil and saltpetre, potassium permanganate reacts in water bath with thermostatic control, water bath with thermostatic control is divided into two stages: maintenance temperature was a certain temperature between 20 ~ 40 degree before this, and the reaction times is 10min ~ 24h; Then add the pure water that volume is soccerballene, the vitriol oil, saltpetre, potassium permanganate mixeding liquid volume 2 ~ 5 times, bath temperature is increased to a certain temperature between 70 ~ 100 degree, is incubated 0 ~ 90 minute.
Removal foreign ion of the present invention, be the method with dialysis, the molecular weight cut-off of dialysis tubing used is 500 ~ 14000.
Drying means of the present invention is Air drying or drying in baking oven, electric furnace, freeze drier.
Accompanying drawing explanation
Fig. 1 is the suspension of obtained graphene quantum dot in the embodiment of the present invention 1;
Fig. 2 is graphene quantum dot powder obtained in the embodiment of the present invention 2;
Fig. 3 is the afm scan figure of graphene quantum dot obtained in the embodiment of the present invention 2;
Fig. 4 is the altitude distribution figure of graphene quantum dot obtained in the embodiment of the present invention 2;
Fig. 5 is the transmission electron microscope figure of graphene quantum dot obtained in the embodiment of the present invention 3;
Fig. 6 is the size distribution plot of graphene quantum dot obtained in the embodiment of the present invention 3.
Embodiment
Below in conjunction with accompanying drawing, further illustrate essentiality content of the present invention with embodiments of the invention, but do not limit the present invention with this.
Embodiment 1
(1) take 0.5g C60 powder, measure the vitriol oil that 10ml massfraction is 98%, C60 powder and the vitriol oil are mixed in beaker, beaker is placed in ice-water bath, stirs with the speed of 100rpm simultaneously.
(2) take 3g potassium permanganate powder, add slowly in the mixed solution in step one.
(3) remove ice-water bath, change water-bath into, keep bath temperature 20 degree, reaction 24h.
(4) 50ml pure water is added fast.
(5) by the suspension filtered that step (4) obtains, then dialyse 3 days with the dialysis tubing that molecular weight cut-off is 8000.
(6) by the suspension Air drying that step (5) obtains, 0.112g graphene quantum dot powder is finally obtained.
Fig. 1 shows the suspension of the graphene quantum dot that step (5) obtains.
Embodiment 2
(1) take 0.5g C60 powder, measure the vitriol oil that 25ml massfraction is 98%, C60 powder and the vitriol oil are mixed in beaker, beaker is placed in ice-water bath, stirs with the speed of 300rpm simultaneously.
(2) take 1.75g potassium permanganate powder, add slowly in the mixed solution in step one.
(3) remove ice-water bath, change water-bath into, keep bath temperature 25 degree, reaction 24h.
(4) 75ml pure water is added fast.
(5) by the suspension filtered that step (4) obtains, then dialyse 7 days with the dialysis tubing that molecular weight cut-off is 500.
(6) suspension step (5) obtained is dry in freeze drier, finally obtains 0.128g graphene quantum dot powder.
Fig. 3 shows the optical photograph of the graphene quantum dot that step (6) obtains; Fig. 4 shows the afm scan figure of graphene quantum dot; Fig. 5 shows the altitude distribution of graphene quantum dot, and it is highly homogeneous is distributed in 1 ~ 2nm.
Embodiment 3
1) take 0.5g C60 powder, measure the vitriol oil that 100ml massfraction is 98%, C60 powder and the vitriol oil are mixed in beaker, beaker is placed in ice-water bath, stirs with the speed of 300rpm simultaneously.
(2) take 0.5g potassium permanganate powder, add slowly in the mixed solution in step one.
(3) remove ice-water bath, change water-bath into, keep bath temperature 40 degree, reaction 1h.
(4) 200ml pure water is added fast.
(5) by the suspension filtered that step (4) obtains, then dialyse 5 days with the dialysis tubing that molecular weight cut-off is 1000.
(6) suspension step (5) obtained is dry in freeze drier, finally obtains 0.108g graphene quantum dot powder.
Fig. 6 shows the transmission electron microscope picture of the graphene quantum dot that step (6) obtains, and show the distribution of sizes of the graphene quantum dot that step (6) obtains, its size uniformity is distributed in 2 ~ 3nm.
Embodiment 4
(1) take 0.5g C70 powder, measure the vitriol oil that 25ml massfraction is 98%, C70 powder and the vitriol oil are mixed in beaker, beaker is placed in ice-water bath, stirs with the speed of 300rpm simultaneously.
(2) take 0.25g SODIUMNITRATE, add in the mixed solution in step one slowly, then take 1.75g potassium permanganate powder, slowly add in mixed solution.
(3) remove ice-water bath, change water-bath into, keep bath temperature 35 degree, reaction 10min.
(4) add 75ml pure water fast, bath temperature is increased to 70 degree, insulation 90min.
(5) by the suspension filtered that step (4) obtains, then dialyse 7 days with the dialysis tubing that molecular weight cut-off is 500.
(6) suspension step (5) obtained is dry in an oven, finally obtains 0.115g graphene quantum dot powder.
Embodiment 5
(1) mixed powder of 0.5g C20, C36, C44, C50, C60, C70, C76, C80, C84, C90, C94, C120, C180, C540 is taken, measure the vitriol oil that 25ml massfraction is 98%, C60 powder and the vitriol oil are mixed in beaker, beaker is placed in ice-water bath, stirs with the speed of 300rpm simultaneously.
(2) take 1.5g SODIUMNITRATE, add slowly in the mixed solution in step one, then take 1.75g potassium permanganate powder.
(3) remove ice-water bath, change water-bath into, keep bath temperature 35 degree, reaction 60min.
(4) add 75ml pure water fast, bath temperature is increased to 100 degree, insulation 90min.
(5) by the suspension filtered that step (4) obtains, then dialyse 7 days with the dialysis tubing that molecular weight cut-off is 500.
(6) suspension step (5) obtained is dry in electric furnace, finally obtains 0.105g graphene quantum dot powder.
To sum up, preparation method of the present invention, from soccerballene, adopts chemical oxidation to cut a step and prepares graphene quantum dot suspension, and the foreign ion in removing suspension, obtains graphene quantum dot powder by drying.Compared with prior art, the preparation method of graphene quantum dot suspension of the present invention and powder solves existing graphene quantum dot suspension and powder preparation method complex process, high in cost of production problem.Preparation method of the present invention is simple to operate, can amplify rapidly and prepare magnanimity graphene quantum dot suspension and powder, have high yield, homogeneous, the water-soluble advantage such as well of the graphene quantum dot distribution of sizes of preparation.
Claims (5)
1. the preparation method of a graphene quantum dot suspension and powder, it is characterized in that, from soccerballene, make graphene quantum dot suspension with chemical oxidation cutting, then remove the foreign ion in suspension, obtain graphene quantum dot powder finally by drying.
2. the preparation method of a kind of graphene quantum dot suspension as claimed in claim 1 and powder, it is characterized in that, described chemical oxidation cutting soccerballene presoma soccerballene and the vitriol oil is mixed in ice-water bath and stirs simultaneously, the consumption of soccerballene and the vitriol oil is the 0.5g soccerballene proportioning vitriol oil 10 ~ 100ml, stirring velocity 100 ~ 1000rpm; Then slowly add SODIUMNITRATE, potassium permanganate, the consumption of SODIUMNITRATE is 0 ~ 3 times of soccerballene quality used, and the consumption of potassium permanganate is 1 ~ 6 times of soccerballene quality used; After potassium permanganate has added, ice-water bath 0 ~ 90min, then changes ice-water bath into water bath with thermostatic control, and temperature is 20 ~ 40 DEG C, insulation 10min ~ 24h; Then add pure water, pure water used be aforementioned soccerballene, the vitriol oil, SODIUMNITRATE, 2 ~ 5 times of potassium permanganate mixeding liquid volume; Bath temperature is warming up to 70 ~ 100 DEG C, insulation 0 ~ 90min.
3. the preparation method of a kind of graphene quantum dot suspension as claimed in claim 1 and powder, it is characterized in that, foreign ion in described removal suspension is that the graphene quantum dot suspension filtered made from chemical oxidation cutting is removed macrobead, the aperture of filter membrane used is 0.01 ~ 0.22um, then dialyse in dialysis tubing, change water every day three times, the molecular weight cut-off of dialysis tubing used is 500 ~ 14000, obtains graphene quantum dot suspension.
4. the preparation method of a kind of graphene quantum dot suspension as claimed in claim 1 and powder, it is characterized in that, described drying be by the suspension Air drying obtained after the foreign ion eliminated in suspension or in baking oven, electric furnace, freeze drier drying obtain graphene quantum dot powder.
5. the preparation method of a kind of graphene quantum dot suspension according to claim 2 and powder, it is characterized in that, described presoma soccerballene is one or more in C20, C36, C44, C50, C60, C70, C76, C80, C84, C90, C94, C120, C180, C540, and described vitriol oil massfraction is 98%.
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