CN107200321A - A kind of method of regulation and control graphene quantum dot luminescence generated by light - Google Patents
A kind of method of regulation and control graphene quantum dot luminescence generated by light Download PDFInfo
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- CN107200321A CN107200321A CN201710445661.9A CN201710445661A CN107200321A CN 107200321 A CN107200321 A CN 107200321A CN 201710445661 A CN201710445661 A CN 201710445661A CN 107200321 A CN107200321 A CN 107200321A
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Abstract
The invention discloses a kind of method of regulation and control graphene quantum dot luminescence generated by light, it is specially:Under ammonia atmosphere, by graphene quantum dot Hg lamp irradiation, by controlling the time of Hg lamp irradiation to realize the photoluminescence property of graphene quantum dot.It is nitrogen source, needs compared with high-temperature and high-pressure conditions regulate and control the method for the characteristics of luminescence of product by preparing doped graphene quantum dot with organic matters such as conventionally employed citric acids, the present invention is using ammonia as nitrogen source, it is the regulation and control that products therefrom (doped graphene quantum dot) characteristics of luminescence can be achieved using photochemical method, technique is more simple and easily manipulates, impurity will not also be introduced, the purity of products therefrom is improved, and the particle diameter distribution of products therefrom is uniform, diameter distribution is about 1 5nm.
Description
Technical field
The present invention relates to graphene quantum dot, and in particular to a kind of method of regulation and control graphene quantum dot luminescence generated by light.
Background technology
Since graphene quantum dot is found, because it has unique electronics, photoelectronic property, graphene quantum
Point has been widely used for many fields such as bio-imaging, luminous and photoelectricity.The particularly adjustable fluorescent material of glow color is in light
There is huge potential application in terms of transmitting, bioluminescence demarcation, Organic Light Emitting Diode and solid state optoelectronic devices.
The method of the regulation and control graphene quantum dot characteristics of luminescence of existing literature report is mostly by synthesizing graphite alkene amount
The solvent of correlation is added during son point, so as to generate doped graphene quantum dot, and then its optical characteristics is regulated and controled.
But these methods normally result in gained doped graphene quantum dot and remain excessive solvent, are unfavorable for application.
The content of the invention
The technical problem to be solved in the present invention is to provide one kind using ammonia as doped source, the regulation and control graphene amount of environmental protection
The method of son point luminescence generated by light.
It is of the present invention regulation and control graphene quantum dot luminescence generated by light method be:Under ammonia atmosphere, by graphene amount
Sub- point Hg lamp irradiation, by controlling the time of Hg lamp irradiation to realize the photoluminescence property of graphene quantum dot.
In above-mentioned technical proposal, the plane and the distance of mercury lamp illumination occurring source where graphene quantum dot is preferably controlled to be
4-9cm, the distance for further preferably control plane where graphene quantum dot and mercury lamp illumination occurring source is 5-7cm.
In above-mentioned technical proposal, the power of the mercury lamp is 300-1000W, preferably 400-600W.
In above-mentioned technical proposal, the ammonia atmosphere generally remains an atmospheric pressure, and the flow of the ammonia is not made especially
It is required that, the application is preferably 40-60ml/min.
In above-mentioned technical proposal, preferably the graphene quantum dot as raw material is placed in quartz boat, then by quartz
Boat is placed in quartz ampoule, above-mentioned quartz ampoule is placed under mercury lamp be again irradiated afterwards.It is preferred that the cross sectional shape of quartz boat is in length
It is square, so it is more beneficial for equably shakeouing graphene quantum dot in quartz boat, is more favorable to graphene quantum dot and exists
Reacted under mercury lamp illumination.Generally, graphene quantum dot spreads thickness control out in 0.05-1mm.
In above-mentioned technical proposal, after irradiation is completed, close ammonia and be passed through inert gas (such as argon gas, helium),
Product is set to be cooled to room temperature in an inert atmosphere.
Applicant in experiments it is found that, using the method for the invention the fluorescence of graphene quantum dot can be realized from gold-tinted
To the Effective Regulation of blue green light, the wherein plane where graphene quantum dot and the distance and mercury lamp of mercury lamp illumination occurring source is shone
The combination for penetrating two parameters of time plays vital effect.Specifically, when the power of mercury lamp is 500W, graphene quantum dot
When the plane at place and the distance of mercury lamp illumination occurring source are that 6cm, irradiation time are 10-90min, the fluorescence of products therefrom can be made
Highest peak is blue shifted to 500-510nm (the fluorescence highest peak of former graphene quantum dot is 551nm).
It is nitrogen source with the organic matter such as conventionally employed citric acid, needs in high-temperature and high-pressure conditions by preparing doped graphene amount
Son point is compared to regulate and control the method for the product characteristics of luminescence, and the present invention, using ammonia as nitrogen source, is that institute can be achieved using photochemical method
The regulation and control of product (doped graphene quantum dot) characteristics of luminescence are obtained, technique is more simple and easily manipulates, and will not also introduce impurity, carry
The high purity of products therefrom, and the particle diameter distribution of products therefrom is uniform, diameter distribution is about 1-5nm.
Brief description of the drawings
Fig. 1 is the transmission electron microscope picture of the raw graphite alkene quantum dot used in each embodiment;
Fig. 2 is the transmission electron microscope picture of the products therefrom of embodiment 4;
Fig. 3 is the fluorescence spectra of the raw graphite alkene quantum dot used in each embodiment;
Fig. 4 is the fluorescence spectra of the products therefrom of embodiment 4;
Fig. 5 is the raw graphite alkene quantum dot that uses in each embodiment, and embodiment 1-5 products therefroms fluorescence spectrum
Figure;
The raw graphite alkene quantum dot used in each embodiments of Fig. 6, and embodiment 1-5 products therefroms X-ray photoelectricity
Sub-light composes (XPS) figure.
Embodiment
With reference to specific embodiment, the present invention is described in further detail, to more fully understand present disclosure, but
The present invention is not limited to following examples.
Transmission electron microscope picture such as Fig. 1 institutes of the raw graphite alkene quantum dot powder (abbreviation GQDs) used in following embodiment
Show, product has relatively uniform dots structure as seen from Figure 1, product diameter is about 1-4nm.Take the raw graphite alkene quantum dot
Powder 1.0mg is dissolved in 10ml deionized waters, then the ultrasound 15min under the conditions of 200W, resulting solution is carried out at room temperature glimmering
Light spectrum test, gained fluorescence spectra is as shown in Figure 3.From the figure 3, it may be seen that the raw material has very strong yellow fluorescence, it is excited
Wavelength has wider scope (280nm-640nm), and the fluorescence intensity when excitation wavelength is 400nm is most strong, and its peak position is
551nm。
Embodiment 1
Take 20mg raw graphite alkene quantum dot powder to be fitted into quartz boat and (spread thickness out for 0.1mm), and quartz boat is put
Enter in quartz ampoule, quartz ampoule is placed in mercury lamp (500W) underface, and control the plane and mercury lamp where graphene quantum dot
The distance of illumination occurring source is 6cm;Backward quartz ampoule in be passed through nitrogen atmosphere (flow is 40ml/min), keep ammonia one
Individual atmospheric pressure, opens mercury lamp and irradiates 10min to graphene quantum dot powder, ammonia is closed after the completion of irradiation, and import argon at once
Gas, allows material to naturally cool to room temperature under argon gas protection, obtains product NGQDs-10 (i.e. nitrogen-doped graphene quantum dots
NGQDs-10)。
Embodiment 2
Embodiment 1 is repeated, unlike, light application time is changed to 30min, product NGQDs-30 is obtained.
Embodiment 3
Embodiment 1 is repeated, unlike, light application time is changed to 50min, product NGQDs-50 is obtained.
Embodiment 4
Embodiment 1 is repeated, unlike, light application time is changed to 70min, product NGQDs-70 is obtained.
Products therefrom NGQDs-70 transmission electron microscope picture is as shown in Fig. 2 product has dots structure, product as seen from Figure 2
Diameter is about 1-5nm.
Products therefrom NGQDs-70 1.0mg are taken to be dissolved in 10ml deionized waters, then the ultrasound 15min under the conditions of 200W, right
Resulting solution carries out fluorescence spectrum test at room temperature, and gained fluorescence spectra is as shown in Figure 4.As shown in Figure 4, the spectrogram with
The fluorescence of raw graphite alkene quantum dot has very big difference, and when excitation wavelength is 400nm, its highest peak appears in 504nm, i.e.,
There is obvious blue shift in the fluorescence of relative raw material graphene quantum dot, and blue green light (504nm) is blue shifted to by gold-tinted (551nm).Say
The band structure of the bright graphene quantum dot under this light application time there occurs obvious change, illustrate this illumination under ammonia atmosphere
Influence of the time to product component is very big.
Embodiment 5
Embodiment 1 is repeated, unlike, light application time is changed to 90min, product NGQDs-90 is obtained.
Embodiment 6
Each 1.0mg of product obtained by Example 1-5 is dissolved in 10ml deionized waters respectively, then ultrasonic under the conditions of 200W
15min, fluorescence spectrum test is carried out to resulting solution at room temperature, and solution after the processing of each embodiment product is excited in 400nm
The fluorescence spectrum of wavelength carries out integration contrast, and result is as shown in Figure 5 after normalization.
As shown in Figure 5, when excitation wavelength is 400nm, the peak position of raw graphite alkene quantum dot is 551nm (gold-tinted),
Exist respectively for 10min, 30min, 50min, 70min, 90min fluorescence highest peak by the method for the invention light application time
508nm (blue green light), 509nm (blue green light), 507nm, 504nm and 510nm (blue green light).As a result show with light application time
Change, its fluorescence all occurs in that obvious blue shift.It follows that can be by selecting light application time in ammonia atmosphere downward arthrolith
The luminous position of black alkene quantum dot, can be realized adjustable from gold-tinted to blue green light.
Embodiment 7
The raw graphite alkene quantum dot used in each embodiment, and embodiment 1-5 products therefroms is taken to carry out XPS tests, spectrum
Figure is as shown in fig. 6, specific data are as described in table 1 below.As a result show that mercury lamp illumination can change gained under ammonia atmosphere to produce
Nitrogen content in thing.
Table 1:
C (%) | N (%) | O (%) | |
GQDs | 62.18 | 1.21 | 36.61 |
NGQDs-10 | 67.91 | 12.28 | 19.81 |
NGQDs-30 | 70.74 | 15.96 | 13.3 |
NGQDs-50 | 71.1 | 14.52 | 14.39 |
NGQDs-70 | 74.37 | 11.41 | 14.22 |
NGQDs-90 | 71.18 | 13.47 | 15.36 |
Embodiment 8
Embodiment 1 is repeated, unlike, ammonia flow is changed to 60ml/min, product NGQDs-10-1 is obtained.
Products therefrom NGQDs-10-1 1.0mg are taken to be dissolved in 10ml deionized waters, then the ultrasound 15min under the conditions of 200W,
Fluorescence spectrum test is carried out at room temperature to resulting solution, fluorescence of the resulting solution in 400nm excitation wavelengths is as a result found most
Strong peak is still 508nm (blue green light).
Embodiment 9
Embodiment 1 is repeated, unlike, plane and the distance of mercury lamp illumination occurring source where control graphene quantum dot
For 7cm, product NGQDs-10-2 is obtained.
Products therefrom NGQDs-10-2 1.0mg are taken to be dissolved in 10ml deionized waters, then the ultrasound 15min under the conditions of 200W,
Fluorescence spectrum test is carried out at room temperature to resulting solution, fluorescence of the resulting solution in 400nm excitation wavelengths is as a result found most
Strong peak is still 508nm (blue green light).
Embodiment 10
Embodiment 1 is repeated, unlike, plane and the distance of mercury lamp illumination occurring source where control graphene quantum dot
For 4cm, product NGQDs-10-3 is obtained.
Products therefrom NGQDs-10-3 1.0mg are taken to be dissolved in 10ml deionized waters, then the ultrasound 15min under the conditions of 200W,
Fluorescence spectrum test is carried out at room temperature to resulting solution, fluorescence of the resulting solution in 400nm excitation wavelengths is as a result found most
Strong peak is still 508nm (blue green light).
Embodiment 11
Embodiment 1 is repeated, unlike, the power of mercury lamp is 1000W, plane and mercury where control graphene quantum dot
The distance that light issues as before source of students is 9cm, obtains product NGQDs-10-4.
Products therefrom NGQDs-10-4 1.0mg are taken to be dissolved in 10ml deionized waters, then the ultrasound 15min under the conditions of 200W,
Fluorescence spectrum test is carried out at room temperature to resulting solution, fluorescence of the resulting solution in 400nm excitation wavelengths is as a result found most
Strong peak is still 508nm (blue green light).
Claims (7)
1. a kind of method of regulation and control graphene quantum dot luminescence generated by light, it is characterised in that:Under ammonia atmosphere, by graphene quantum
Point Hg lamp irradiation, by controlling the time of Hg lamp irradiation to realize the photoluminescence property of graphene quantum dot.
2. according to the method described in claim 1, it is characterised in that:Plane where graphene quantum dot occurs with mercury lamp illumination
The distance in source is 4-9cm.
3. method according to claim 2, it is characterised in that:Plane where graphene quantum dot occurs with mercury lamp illumination
The distance in source is 5-7cm.
4. according to the method described in claim 1, it is characterised in that:The power of the mercury lamp is 300-1000W.
5. method according to claim 4, it is characterised in that:The power of the mercury lamp is 400-600W.
6. according to the method described in claim 1, it is characterised in that:The ammonia atmosphere keeps an atmospheric pressure.
7. the method according to any one of claim 1-6, it is characterised in that:When the power of mercury lamp is 500W, graphene
, can be by products therefrom when plane where quantum dot and the distance of mercury lamp illumination occurring source are that 6cm, irradiation time are 10-90min
Fluorescence highest peak be blue shifted to 500-510nm.
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Cited By (3)
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CN108314005A (en) * | 2018-03-27 | 2018-07-24 | 广西师范大学 | A kind of method and its device preparing chlorine doped graphene quantum dot |
CN108706579A (en) * | 2018-07-23 | 2018-10-26 | 广西师范大学 | A method of preparing Fluorin doped graphene quantum dot |
CN114479847A (en) * | 2022-02-18 | 2022-05-13 | 广西师范大学 | Graphene oxide quantum dot emitting purple fluorescence and preparation method thereof |
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Cited By (4)
Publication number | Priority date | Publication date | Assignee | Title |
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CN108314005A (en) * | 2018-03-27 | 2018-07-24 | 广西师范大学 | A kind of method and its device preparing chlorine doped graphene quantum dot |
CN108706579A (en) * | 2018-07-23 | 2018-10-26 | 广西师范大学 | A method of preparing Fluorin doped graphene quantum dot |
CN114479847A (en) * | 2022-02-18 | 2022-05-13 | 广西师范大学 | Graphene oxide quantum dot emitting purple fluorescence and preparation method thereof |
CN114479847B (en) * | 2022-02-18 | 2023-09-22 | 广西师范大学 | Purple fluorescent graphene oxide quantum dot and preparation method thereof |
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