CN104556004A - Preparation method of controlled fluorescent graphene quantum dot - Google Patents
Preparation method of controlled fluorescent graphene quantum dot Download PDFInfo
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- CN104556004A CN104556004A CN201410828364.9A CN201410828364A CN104556004A CN 104556004 A CN104556004 A CN 104556004A CN 201410828364 A CN201410828364 A CN 201410828364A CN 104556004 A CN104556004 A CN 104556004A
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Abstract
The invention discloses a preparation method of a controlled fluorescent graphene quantum dot. The preparation method comprises the following steps: uniformly and quickly dispersing graphite oxide into ultrapure water by ultrasonic action to obtain a dispersion liquid of graphite oxide; adding different amount of hydrogen peroxide solution into the obtained dispersion liquid of graphite oxide, and at last, obtaining the graphene quantum dot under ultraviolet radiation. The preparation method disclosed by the invention is simple, and short in technology process; the prepared product is small in particle size, uniform in distribution, and excellent in fluorescent property; the conditions can be controlled to prepare the graphene quantum dot with the required wavelength.
Description
Technical field
The invention belongs to technical field of nanometer material preparation, be specifically related to a kind of preparation method of controllable fluorescent graphene quantum dot.
Background technology
Graphene (GQDs) be a kind of by carbon atom with SP
2the hexagonal carbon material of hybridized orbital composition, thickness is only the monoatomic thickness of one deck.Graphene quantum dot not only has outside the advantages such as the hardness of Graphene is strong, thermal conductivity is high, electronic mobility is fast, resistivity is low, when its size is less than 10nm, also has new physical properties because of quantum confined effect and side effect.So graphene quantum dot is widely used in imaging biological cells, biomarker, electrochemical sensing, nano-electrode etc.
In prior art, graphene preparation method is various, sums up and gets up to have two large classes: from top to bottom and from bottom to top.Top-to-bottom method refers to, by physics or chemical process, large-sized graphene platelet is cut into undersized graphene quantum dot, comprises hydrothermal method, electrochemical process, chemical stripping method, ultrasonic method and microwave method etc.; Bottom-to-top method then refers to using small molecules prepares graphene quantum dot as precursor by series of chemical.These two large class methods respectively have quality, and top-to-bottom method step is simple, and productive rate is higher, but can not realize the pattern of graphene quantum dot and the accurate control of size; Bottom-to-top method controllability is strong, but complex steps, troublesome poeration.
Summary of the invention
For solving the technical problem of existing existence, the embodiment of the present invention provides a kind of preparation method of controllable fluorescent graphene quantum dot.
For achieving the above object, the technical scheme of the embodiment of the present invention is achieved in that
The embodiment of the present invention provides a kind of preparation method of controllable fluorescent graphene quantum dot, and this preparation method is: be dispersed in evenly and rapidly in ultrapure water by graphite oxide by ultrasonication, obtains the dispersion liquid of graphite oxide; In the dispersion liquid of the graphite oxide of described acquisition, add superoxol, finally under ultraviolet radiation, obtain graphene quantum dot.
In such scheme, the concentration of the dispersion liquid of the graphite oxide of described acquisition is 20 μ g/mL to 150 μ g/mL.
In such scheme, described ultrasonication is specially to be carried out on Ultrasonic Cleaners, and power is 100W, ultrasonic treatment time 10min to 60min.
In such scheme, the volume fraction 1% ~ 10% of hydrogen peroxide in described superoxol.
In such scheme, describedly under ultraviolet radiation, be specially radiation under high-pressure mercury vapor Jupiter, below distance high-voltage mercury vapour Jupiter, uv irradiating is carried out in the place of 10cm, radiated time 5min to 60min.
Compared with prior art, beneficial effect of the present invention:
Present invention incorporates these two advantages of chemical chop effect of ultrasonic stripping effect and advanced oxidation, and preparation process can carry out chemical chop to graphite oxide without the need to the participation of ferrous ion, avoid being mixed into of impurity, without the need to follow-up dialysis procedure, prevent iron ion to the cancellation effect of graphene quantum dot fluorescence; Preparation method is simple, and technical process is short, and it is little and be evenly distributed that the product of preparation has particle diameter, and photoluminescent property is excellent, and can by the graphene quantum dot of the required wavelength of control condition preparation.
Accompanying drawing explanation
The schematic flow sheet of the preparation method of a kind of controllable fluorescent graphene quantum dot that Fig. 1 provides for the embodiment of the present invention;
Fig. 2 is the transmission electron microscope picture of graphene quantum dot prepared by the embodiment of the present invention 1;
Fig. 3 is the fluorescence spectrum figure of graphene quantum dot prepared by the embodiment of the present invention 1,2,3;
The Raman spectrum of Fig. 4 to be the embodiment of the present invention 3 radiated time be graphene quantum dot of 30min;
Fig. 5 is the embodiment of the present invention 4, the fluorescence spectrum figure of the graphene quantum dot of 5,6 preparations.
Embodiment
Below in conjunction with the drawings and specific embodiments, the present invention is described in detail.
The embodiment of the present invention provides a kind of preparation method of controllable fluorescent graphene quantum dot, and as shown in Figure 1, this preparation method is realized by following steps:
Step 101: prepare the graphite oxide aqueous solution.
Concrete, by ultrasonication, graphite oxide is dispersed in ultrapure water evenly and rapidly, obtains the dispersion liquid of graphite oxide; The concentration of the dispersion liquid of the graphite oxide of described acquisition is 20 μ g/mL to 150 μ g/mL.
Described ultrasonication is specially to be carried out on Ultrasonic Cleaners, and power is 100W, ultrasonic treatment time 10min to 60min.Described ultrapure water is that the resistivity prepared through Milli Q water purification machine reaches 18.2M Ω cm
-1ultrapure water.Described graphite oxide prepares with reference to Hummers method, and the quality of described graphite oxide is 0.0030g to 0.0225g, is dispersed in 20mL ultrapure water.
Described Ultrasonic Cleaners also can adopt other ultrasonic devices, and power is 100W, and watt level is adjustable, if the power selected is large, then corresponding ultrasonic time shortens; Vice versa.
Step 102: prepare graphene quantum dot.
Concrete, in the dispersion liquid of the graphite oxide of described acquisition, add superoxol, finally under ultraviolet radiation, obtain graphene quantum dot.
The volume fraction 30% of described superoxol, get described superoxol 5mL to 50mL respectively, add in the graphite oxide dispersion of step 101 preparation, then add ultrapure water, make the cumulative volume of this dispersion liquid be 150mL, and wherein the volume fraction of hydrogen peroxide is 1% to 10%.
Describedly under ultraviolet radiation, be specially radiation under high-pressure mercury vapor Jupiter (1KW), below distance high-voltage mercury vapour Jupiter, uv irradiating is carried out in the place of 10cm, radiated time 5min to 60min, consumption and the UV irradiation time of size and hydrogen peroxide are directly proportional.When radiated time is 30min, particle diameter is little and even, and during more than 30min, graphene quantum dot, in hydroxyl radical free radical effect cutting, finally can become carbonic acid gas, and can not obtain target product---graphene quantum dot.
The optional kapillary extra-high-pressure mercury vapour lamp of fluorescent tube of described mercury vapour Jupiter or plate burning light etc. can produce ultraviolet equipment, if select certain specific fluorescent tube, supporting barretter and triggering device is then needed to use, power 1KW, the watt level of lamp can select 2KW, 5KW, 8KW, if select high-power fluorescent tube, then shorten the radiated time of graphite oxide is also corresponding.
Describedly carry out uv irradiating from the place of 10cm below high-pressure mercury vapor Jupiter, apart from adjustable 5-25cm, radiation length increases, then radiated time needs to extend.
The monodispersity of the graphene quantum dot obtained by aforesaid method is good, and particle diameter is little, is evenly distributed, good water solubility, has strong fluorescence property.
Embodiment 1
Take 0.0150g graphite oxide, add the ultrapure water of 20mL.Supersound process 30min, then adds hydrogen peroxide (30%) 5mL, then adds ultrapure water 125mL, then radiation under high-pressure mercury vapor Jupiter.Sample portion before irradiation, and radiated time is that 5min, 10min, 15min, 20min, 25min, 30min, 45min, 60min respectively materials portion, this serial solution is the graphene quantum dot of preparation.
As shown in Figure 2, A, B, C, D, E, F in Fig. 2 are radiated time is respectively 5min, 10min, 15min, 20min, 25min, 30min; When radiated time is 5min, the particle diameter of GQDs is still larger; When irradiation time lengthens is to 30min, the diameter of GQDs is only 5nm, and even particle size distribution.
Embodiment 2
Take 0.0150g graphite oxide, add the ultrapure water of 20mL.Supersound process 30min, then adds hydrogen peroxide (30%) 25mL, then the 105mL that adds water, then radiation under high-pressure mercury vapor Jupiter.Sample portion before irradiation, and radiated time is that 5min, 10min, 15min, 20min, 25min, 30min, 45min, 60min respectively materials portion, this serial solution is the graphene quantum dot of preparation.
Embodiment 3
Take 0.0150g graphite oxide, add the ultrapure water of 20mL.Supersound process 30min, then adds hydrogen peroxide (30%) 50mL, then the 80mL that adds water, then radiation under high-pressure mercury vapor Jupiter.Sample portion before irradiation, and radiated time is that 5min, 10min, 15min, 20min, 25min, 30min, 45min, 60min respectively materials portion, this serial solution is the graphene quantum dot of preparation.
As shown in Figure 3, A, B, C in Fig. 3 are embodiment 1 respectively, the fluorescence spectrum figure of the graphene quantum dot of 2,3 preparations; Visible, the GQDs obtained under different radiated time, generally there is blue-shifted phenomenon in its fluorescence maximum wavelength, when excitation wavelength is 370nm, the maximum emission wavelength of GQDs moves to 500nm (60min) by 650nm (0min); During radiated time 30min, fluorescence intensity is the strongest, and now maximum emission wavelength is at 550nm.D in Fig. 3 is graphene quantum dot obtained when radiated time is 30min in embodiment 3, the situation that its fluorescence emission spectrum changes with different excitation wavelength; Visible, fluorescence emission wavelengths does not move with excitation wavelength substantially, and just intensity changes.
As shown in Figure 4, Fig. 4 is embodiment 3, under different radiated time, and the Raman spectrogram of the graphene quantum dot prepared.As seen from the figure, along with the increase of radiated time, two characteristic peaks (D peak and G peak, the i.e. sp of defect peak and carbon atom of graphene quantum dot in Raman spectrum
2hybrid characteristics peak) position substantially do not change, and the ratio of two peak intensities presents regular change.Reaction is initial, D peak intensity and G peak intensity all smaller; Along with the carrying out of reaction, its intensity ratio (D/G) increases gradually, and during radiation 30min, ratio reaches maximum, and then then presents reduction trend.Above result shows, in radiative process, the OH that under action of ultraviolet light, hydrogen peroxide produces causes defect on graphite oxide surface; Reaction proceeds to a certain degree, after graphite oxide is cut into graphene quantum dot, and this defect structure in quantum dot and graphene-structured (sp
2hydridization) tend to balance.
Embodiment 4
Take 0.0150g graphite oxide, add the ultrapure water of 20mL.Supersound process 10min, then adds hydrogen peroxide (30%) 5mL, then the 125mL that adds water, high-pressure mercury vapor Jupiter radiation 1h.Sample before irradiation, be then that 5min, 10min, 15min, 20min, 25min, 30min, 45min, 60min respectively materials portion at radiated time, this serial solution is the graphene quantum dot of preparation.
Embodiment 5
Take 0.0150g graphite oxide, add the ultrapure water of 20mL.Supersound process 30min, then adds hydrogen peroxide (30%) 5mL, then the 125mL that adds water.High-pressure mercury vapor Jupiter radiation 1h.Sample before irradiation, be then that 5min, 10min, 15min, 20min, 25min, 30min, 45min, 60min respectively materials portion at radiated time, this serial solution is the graphene quantum dot of preparation.
Embodiment 6
Take 0.0150g graphite oxide, add the ultrapure water of 20mL.Supersound process 60min, then adds hydrogen peroxide (30%) 5mL, then the 125mL that adds water, high-pressure mercury vapor Jupiter radiation 1h.Sample before irradiation, be then 5min, 10min, 15min, 20min, 25min, 30min, 45min, 60min at radiated time, this serial solution is the graphene quantum dot of preparation.
As shown in Figure 5, A, B, C in Fig. 5 are respectively embodiment 4, the fluorescence spectrum figure of the graphene quantum dot of 5,6 preparations; When under the condition that the hydrogen peroxide volume integral number that graphite oxide dispersion concentration is identical, add is identical, the graphene quantum dot that the different ultrasonic disperse time obtains.Visible, the fluorescence spectrum of time on obtained graphene quantum dot of ultrasonic disperse graphite oxide has impact.In Fig. 5 A, along with radiated time is increased to 60min from 0min, the fluorescent emission peak position of graphene quantum dot, by 650nm, moves to 520nm place, finally move to 500nm place, and the strongest fluorescent emission appears at 650nm; The wavelength of fluorescence Changing Pattern of Fig. 5 B and Fig. 5 A is similar, and just maximum fluorescence emission wavelengths is 520nm; In Fig. 5 C, the fluorescent emission peak position of graphene quantum dot moves to 450nm by 650nm, and does not occur fluorescence emission peak at 520nm place.
Claims (5)
1. a preparation method for controllable fluorescent graphene quantum dot, is characterized in that, this preparation method is: be dispersed in evenly and rapidly in ultrapure water by graphite oxide by ultrasonication, obtains the dispersion liquid of graphite oxide; In the dispersion liquid of the graphite oxide of described acquisition, add superoxol, finally under ultraviolet radiation, obtain graphene quantum dot.
2. the preparation method of controllable fluorescent graphene quantum dot according to claim 1, is characterized in that: the concentration of the dispersion liquid of the graphite oxide of described acquisition is 20 μ g/mL to 150 μ g/mL.
3. the preparation method of controllable fluorescent graphene quantum dot according to claim 1 and 2, is characterized in that: described ultrasonication is specially to be carried out on Ultrasonic Cleaners, and power is 100W, ultrasonic treatment time 10min to 60min.
4. the preparation method of controllable fluorescent graphene quantum dot according to claim 3, is characterized in that: the volume fraction 1% ~ 10% of hydrogen peroxide in described superoxol.
5. the preparation method of controllable fluorescent graphene quantum dot according to claim 4, it is characterized in that: describedly under ultraviolet radiation, be specially radiation under high-pressure mercury vapor Jupiter, below distance high-voltage mercury vapour Jupiter, uv irradiating is carried out in the place of 10cm, radiated time 5min to 60min.
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Cited By (14)
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| CN105502369A (en) * | 2015-12-31 | 2016-04-20 | 北京科技大学 | Post redox treatment method for adjusting photoluminescent property of graphene quantum dots |
| CN105565302A (en) * | 2015-12-23 | 2016-05-11 | 西安电子科技大学 | Method for preparation of graphene quantum dots on the basis of hypochlorite radical oxidation |
| CN106348281A (en) * | 2015-07-13 | 2017-01-25 | 南京理工大学 | Method for preparing bifluorescence graphene quantum dots hydrothermally |
| WO2017032330A1 (en) * | 2015-08-25 | 2017-03-02 | 深圳粤网节能技术服务有限公司 | Preparation method for graphene quantum dots with different oxygen content, graphene quantum dot, and fluorescent material |
| CN106629649A (en) * | 2015-07-13 | 2017-05-10 | 南京理工大学 | One-step solvothermal method for preparing strong fluorescence graphene quantum dots |
| CN106672957A (en) * | 2016-07-18 | 2017-05-17 | 中国科学院兰州化学物理研究所 | Method for preparing graphene oxide according to Fenton oxidation method |
| CN107098336A (en) * | 2017-04-28 | 2017-08-29 | 成都川烯科技有限公司 | A kind of method that graphene quantum dot is prepared based on photochemical method |
| CN107200321A (en) * | 2017-06-13 | 2017-09-26 | 广西师范大学 | A kind of method of regulation and control graphene quantum dot luminescence generated by light |
| CN107758643A (en) * | 2016-08-16 | 2018-03-06 | 中国科学院宁波材料技术与工程研究所 | Graphene quantum dot, its preparation method and application |
| CN108190877A (en) * | 2018-02-22 | 2018-06-22 | 国家纳米科学中心 | A kind of graphene oxide, preparation method and purposes |
| CN108842157A (en) * | 2018-02-08 | 2018-11-20 | 浙江工业大学 | A method of multicolor fluorescence graphene quantum dot is prepared in same electrolytic tank electrolysis |
| CN111427111A (en) * | 2020-03-30 | 2020-07-17 | Tcl华星光电技术有限公司 | Quantum dot patterning method, device and system |
| US11377723B2 (en) | 2020-03-30 | 2022-07-05 | Tcl China Star Optoelectronics Technology Co., Ltd. | Method of patterning quantum dots, device using same, and system thereof |
| CN115924896A (en) * | 2022-12-26 | 2023-04-07 | 上海纳米技术及应用国家工程研究中心有限公司 | Method for preparing graphene quantum dots by using heterogeneous catalyst |
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| CN106629649A (en) * | 2015-07-13 | 2017-05-10 | 南京理工大学 | One-step solvothermal method for preparing strong fluorescence graphene quantum dots |
| CN106348281A (en) * | 2015-07-13 | 2017-01-25 | 南京理工大学 | Method for preparing bifluorescence graphene quantum dots hydrothermally |
| US11299671B2 (en) | 2015-08-25 | 2022-04-12 | Linde ZHANG | Preparation method for graphene quantum dots with different oxygen contents, graphene quantum dot, and fluorescent material |
| WO2017032330A1 (en) * | 2015-08-25 | 2017-03-02 | 深圳粤网节能技术服务有限公司 | Preparation method for graphene quantum dots with different oxygen content, graphene quantum dot, and fluorescent material |
| CN105565302B (en) * | 2015-12-23 | 2018-01-12 | 西安电子科技大学 | The method for carrying out graphene quantum dot preparation is aoxidized based on hypochlorite |
| CN105565302A (en) * | 2015-12-23 | 2016-05-11 | 西安电子科技大学 | Method for preparation of graphene quantum dots on the basis of hypochlorite radical oxidation |
| CN105502369A (en) * | 2015-12-31 | 2016-04-20 | 北京科技大学 | Post redox treatment method for adjusting photoluminescent property of graphene quantum dots |
| CN105502369B (en) * | 2015-12-31 | 2018-02-02 | 北京科技大学 | Adjust the rear oxidation method of reduction treatment of graphene quantum dot photoluminescence performance |
| CN106672957A (en) * | 2016-07-18 | 2017-05-17 | 中国科学院兰州化学物理研究所 | Method for preparing graphene oxide according to Fenton oxidation method |
| CN107758643A (en) * | 2016-08-16 | 2018-03-06 | 中国科学院宁波材料技术与工程研究所 | Graphene quantum dot, its preparation method and application |
| CN107098336A (en) * | 2017-04-28 | 2017-08-29 | 成都川烯科技有限公司 | A kind of method that graphene quantum dot is prepared based on photochemical method |
| CN107200321A (en) * | 2017-06-13 | 2017-09-26 | 广西师范大学 | A kind of method of regulation and control graphene quantum dot luminescence generated by light |
| CN108842157A (en) * | 2018-02-08 | 2018-11-20 | 浙江工业大学 | A method of multicolor fluorescence graphene quantum dot is prepared in same electrolytic tank electrolysis |
| CN108190877A (en) * | 2018-02-22 | 2018-06-22 | 国家纳米科学中心 | A kind of graphene oxide, preparation method and purposes |
| CN111427111A (en) * | 2020-03-30 | 2020-07-17 | Tcl华星光电技术有限公司 | Quantum dot patterning method, device and system |
| US11377723B2 (en) | 2020-03-30 | 2022-07-05 | Tcl China Star Optoelectronics Technology Co., Ltd. | Method of patterning quantum dots, device using same, and system thereof |
| CN115924896A (en) * | 2022-12-26 | 2023-04-07 | 上海纳米技术及应用国家工程研究中心有限公司 | Method for preparing graphene quantum dots by using heterogeneous catalyst |
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