CN103553026A - Method for preparing purple fluorescence reduced oxidized graphene quantum dot - Google Patents
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- CN103553026A CN103553026A CN201310478343.4A CN201310478343A CN103553026A CN 103553026 A CN103553026 A CN 103553026A CN 201310478343 A CN201310478343 A CN 201310478343A CN 103553026 A CN103553026 A CN 103553026A
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Abstract
The invention discloses a method for preparing purple fluorescence reduced oxidized graphene quantum dot. According to the method, oxidized graphene, which is used as a raw material, is subjected to oxidation treatment by the use of nitric acid and sulfuric acid; an oxidized graphene solution which has been oxidized is subjected to ultrasonic decomposition by the use of a 200W ultrasonic machine for 14 hours; the solution is subjected to deacidification and cleaning by a centrifugal separation process at the rotating speed of 14000 r/m until pH value of the solution is adjusted to 8; high-pressure digestion is conducted at 200 DEG C for 12 hours; the solution which has undergone digestion is subjected to continuous dialysis by the use of a 8000-14000Da dialysis bag for about one week; the solution is dried in vacuum at 90 DEG C so as to obtain oxidized graphene quantum dot; the oxidized graphene quantum dot is reduced in the H2 atmosphere at 300-900 DEG C for 1 hour; and hydrogen is turned off, argon is introduced immediately, and a tubular furnace is naturally cooled to room temperature so as to obtain the reduced oxidized graphene quantum dot. According to the invention, any impure impurity materials are not added such that the prepared product has high purity; particle size distribution is uniform; and fluorescence can be adjusted from blue light to purple light.
Description
Technical field
The present invention relates to a kind of redox graphene quantum dot with purple fluorescence and preparation method thereof.
Background technology
Since graphene quantum dot is found, because it has unique electronics, photoelectronic property, graphene quantum dot has been widely used in many fields such as bio-imaging, luminous and photoelectricity.There is huge potential application in the blue fluorescent material to purple particularly aspect light emission, bioluminescence demarcation, Organic Light Emitting Diode and solid-state light electrical part.Yet the graphene quantum dot of report shows as green or blue fluorescence mostly at present.Redox graphene quantum dot prepared by present method has obvious purple fluorescence feature, and the position at fluorescence radiation peak by experiment condition effectively regulates, be that green or blue the strong of fluorescence graphene quantum dot of current traditional method preparation supplements, can expand the application of graphene quantum dot aspect photoelectric material.
Summary of the invention
The object of the invention is to, propose a kind of preparation method of new purple fluorescence redox graphene quantum dot.The present invention cleans the graphene oxide after oxide treatment by the method for using deionized water to carry out high speed centrifugation separation.Compare with traditional method, technique of the present invention does not add in the alkaline matters such as any sodium hydroxide and the graphene oxide solution of oxide treatment.Therefore, technique of the present invention has the feature that does not add any impure impurity material.And this preparation technology is simple, process is easily controlled, suitable for mass production.
Technical scheme of the present invention is: prepare the method for purple fluorescence redox graphene quantum dot, it is characterized in that comprising the steps:
(1) take graphene oxide as starting material, using nitric acid, sulfuric acid as oxygenant, the ratio that adds 25ml-35ml nitric acid, 5ml-15ml sulfuric acid with every 50mg graphene oxide carries out invading for 20-30 hour bubble oxide treatment to graphene oxide;
(2) the graphene oxide solution after oxidation in step (1) is carried out to 10-18 hour ultrasonic decomposition;
(3) utilize the graphene oxide solution after ultrasonic in deionized water dilution step (2);
(4) the graphene oxide solution after dilution in step (3) being carried out repeatedly to centrifugal disacidify processes;
(5) graphene oxide after utilizing deionized water to disacidify in step (4) carries out eccentric cleaning 10-15 time, until solution ph is adjusted to 8;
(6) gained solution in step (5) is carried out to high-pressure digestion 10-14 hour at 200 ± 20 ℃;
(7) dialysis tubing of the soln using 8000～14000Da after clearing up in step (6) is carried out to the continuous dialysis of 5-10 days;
(8) collect the solution of dialysing outside back pkt. continuously in step (7), under 90 ± 5 ℃ of conditions, carry out drying and processing; Especially in described step (8), introduce 200Pa with dry under interior pressure;
(9) by drying gained graphene oxide quantum dot powder in step (8), pack quartz boat into and put into silica tube, at H
2lower 300 ℃ of-900 ℃ of thermal reduction 40-80 minute of atmosphere, close hydrogen, import at once argon gas, allow silica tube naturally cool to room temperature, obtain redox graphene quantum dot.
Further, described step (1) be take graphene oxide as starting material, usings nitric acid, sulfuric acid as oxygenant, and the ratio that adds 30ml nitric acid, 10ml sulfuric acid with every 50mg graphene oxide carries out invading for 24 hours bubble oxide treatment to graphene oxide.
Further, in step (2), utilize the ultrasonic machine of 200W that the graphene oxide solution after oxidation in step (1) is carried out to 10-18 hour ultrasonic decomposition.
Further, the graphene oxide solution after ultrasonic in step (2) is that 1-1.5:5 mixes with deionized water described in step (3) according to volume ratio, the graphene oxide solution after ultrasonic in dilution step (2).
Further, utilize high speed freezing centrifuge to adopt the rotating speed of 10000-18000 rev/min to carry out repeatedly time disacidify to the graphene oxide solution after diluting in step (3) and process in step (4), each centrifugation time is 30-50 minute.
Further, the graphene oxide in step (4) after disacidify is that 1-1.5:5 mixes with deionized water described in step (5) according to mass ratio, carries out eccentric cleaning 10-15 time, until solution ph is adjusted to 8.
Further, in step (6), gained soln using high-pressure digestion tank in step (5) is carried out to high-pressure digestion 10-14 hour at 200 ± 20 ℃.
Further, H in described step (9)
2flow be 100sccm-200sccm.
Further, in described step (9), in silica tube, make H
2remain on a normal atmosphere.
The invention has the beneficial effects as follows: in existing graphene quantum dot preparation method, conventionally add sodium hydroxide to regulate the ph value of corresponding solution, this has introduced impurity virtually, and this,, by affecting the purity of graphene quantum dot, brings impact to practical application.The present invention cleans the graphene oxide after oxide treatment by the method for using deionized water to carry out high speed centrifugation separation, do not add any impure impurity material, graphene oxide quantum dot and the redox graphene quantum dot purity of preparation are high, and size distribution is even, is generally about 1～6 nanometer.Meanwhile, the fluorescence of redox graphene quantum dot prepared by method of the present invention has the adjustability from blue light to purple light, and regulation range is blue shifted to 407 nanometers from 441 nanometers.
The product of preparing with the present invention carries out structure and performance characterization by following means: the shape and size that the JEM-200 CX transmission electron microscope (TEM) that utilizes Japanese JEOL company to produce is directly observed product; Adopt fluorescence spectrophotometer, the fluorescence situation of analytic sample.
Accompanying drawing explanation
Fig. 1 is the typical transmission electron microscope observed result of the graphene oxide quantum dot of embodiment 1 preparation;
Fig. 2 is the transmission electron microscope observed result of the redox graphene quantum dot rGOQDs-300 of embodiment 2 preparations;
Fig. 3 is the transmission electron microscope observed result of the redox graphene quantum dot rGOQDs-600 of embodiment 3 preparations;
Fig. 4 is the transmission electron microscope observed result of the redox graphene quantum dot rGOQDs-900 of embodiment 4 preparations;
Fig. 5 is the fluorescence spectrum figure of the graphene oxide quantum dot of embodiment 1 preparation;
Fig. 6 is in example 4 preparation process, the fluorescence result figure of the redox graphene quantum dot rGOQDs-900 that annealing obtains at 900 ℃ of temperature;
Fig. 7 is the fluorescence spectrum result of the sample of example 7 tests.
Wherein, rGOQDs-300, rGOQDs-600, rGOQDs-900 are the name of gained sample, numeral annealing temperature.
Embodiment
Below in conjunction with accompanying drawing, the specific embodiment of the present invention is further described, in embodiment, agents useful for same is chemical pure.
Embodiment 1: prepare the method for graphene oxide quantum dot, comprise the steps:
(1) take graphene oxide as starting material, using nitric acid, sulfuric acid as oxygenant, 150mg graphene oxide is dissolved in the nitric acid of 75ml, 90ml or 105ml and the sulphuric acid soln of 15ml, 30ml or 45ml, under normal temperature, invades bubble 20 hours, 24 hours or 30 hours oxide treatment; Wherein to invade 24 hours oxide treatment better effects if of bubble under the nitric acid of 90ml and the sulphuric acid soln normal temperature of 30ml.
(2) utilize the ultrasonic machine of 200W that the graphene oxide solution after oxidation in step (1) is carried out 10 hours, 14 hours or 18 hours ultrasonic decomposition; Result shows that the ultrasonic decomposition effect of 14 hours is best, surpasses the ultrasonic decomposition of 14 hours to not significantly impact of experimental result.
(3) the graphene oxide solution after ultrasonic in step (2) is transferred in beaker, and adds the deionized water of 500ml, 600ml or 700ml to dilute; The deionized water dilution effect of 600ml is best.
(4) adopt the rotating speed of 14000 revs/min to carry out repeatedly centrifugal disacidify the soln using high speed freezing centrifuge after dilution in step (3) and process, each centrifugation time is 30-50 minute;
(5) graphene oxide after utilizing deionized water to disacidify in step (4) is that 1-1.5:5 carries out 10-15 time eccentric cleaning again according to mass ratio, until ph=8; Wherein in deionized water and step (4), the graphene oxide after disacidify is according to mass ratio 4:1 eccentric cleaning, and fastest, effect is best.
(6) gained soln using high-pressure digestion tank in step (5) is carried out to high-pressure digestion 10 hours, 12 hours or 14 hours at 180 ℃, 200 ℃ or 220 ℃, wherein carry out high-pressure digestion 10 hours, 12 hours at 180 ℃, 200 ℃ or 220 ℃ or 14 hours effects without remarkable difference.
(7) gained solution in step (6) is put in the dialysis tubing of 8000～14000Da, and added in addition magnetic agitation of deionized water, carry out the continuous dialysis of 5-10 days.
(8) collect the solution in beaker in step (7), under vacuum and 90 ± 5 ℃ of conditions, carry out being cooled to room temperature after drying and processing the graphene oxide quantum dot powder obtaining.Repeat this scheme and obtain more graphene oxide quantum dot.Sample transmission electron microscope observed result is shown in Fig. 1.
Embodiment 2: 10mg graphene oxide quantum dot powder is packed into quartz boat and puts into silica tube, is the H of 100sccm or 200sccm at flow
2in atmosphere, remain under a normal atmosphere, carry out after heat reduction, importing at once argon gas and closing hydrogen for 1 hour in 300 ℃, allow silica tube naturally cool to room temperature, the transmission electron microscope observed result that obtains redox graphene quantum dot rGOQDs-300 is shown in Fig. 2.The H of 100sccm or 200sccm wherein
2flow experiment effect is without remarkable difference.
Embodiment 3: in the same manner as in Example 2, but reduction temperature changes 600 ℃ into for experimentation and condition, and the transmission electron microscope observed result that obtains redox graphene quantum dot rGOQDs-600 is shown in Fig. 3.
Embodiment 4: in the same manner as in Example 2, but reduction temperature changes 900 ℃ into for experimentation and condition, and the transmission electron microscope observed result that obtains redox graphene quantum dot rGOQDs-900 is shown in Fig. 4.
Embodiment 5: embodiment 1 is prepared to gained graphene oxide quantum dot 1.0mg and be dissolved in 20ml deionized water, then supersound process 1 hour under 200W condition, at room temperature carries out fluorescence spectrum test to gained solution, and gained fluorescence spectrum figure is shown in Fig. 4.
Embodiment 6: embodiment 4 is prepared to gained redox graphene quantum dot according to the process of embodiment 5 and condition is processed and fluorometric investigation, acquired results is shown in Fig. 6.
Embodiment 7: embodiment 2, embodiment 3 with embodiment 4 prepares gained redox graphene quantum dot according to the process of embodiment 5 and condition is processed and fluorometric investigation, found that blue shift has all appearred in its fluorescence, and all when being 300nm, excitation wavelength there is hyperfluorescenceZeng Yongminggaoyingguang peak, therefore embodiment 1 to embodiment 6 gained sample is integrated to contrast at the fluorescence spectrum of 300nm excitation wavelength, the results are shown in Figure 7.
Fig. 1 is the typical transmission electron microscope observed result of the graphene oxide quantum dot of embodiment 1 preparation, and product has dots structure relatively uniformly as seen from the figure.Product diameter is about 1～6 nanometer.
Fig. 2 is the transmission electron microscope observed result of the redox graphene quantum dot rGOQDs-300 of embodiment 2 preparations, and product has dots structure relatively uniformly equally as seen from the figure.Product diameter is about 1～6 nanometer.
Fig. 3 is the transmission electron microscope observed result of the redox graphene quantum dot rGOQDs-600 of embodiment 3 preparations, and product has dots structure relatively uniformly equally as seen from the figure.Product diameter is about 1～6 nanometer.
Fig. 4 is the transmission electron microscope observed result of the redox graphene quantum dot rGOQDs-900 of embodiment 4 preparations, and product has dots structure relatively uniformly equally as seen from the figure.Product diameter is about 1～6 nanometer.
Fig. 5 is the fluorescence spectrum figure of the graphene oxide quantum dot of embodiment 1 preparation, as can be seen from the figure, the blue-fluorescence that the existence of this sample is very strong, its excitation wavelength has wider scope (260nm-440nm), fluorescence intensity when excitation wavelength is 320nm is the strongest, and its peak position is 441nm.
Fig. 6 is in example 4 preparation process, the fluorescence result figure of the redox graphene quantum dot rGOQDs-900 that annealing obtains at 900 ℃ of temperature, the fluorescence that found that this spectrogram and graphene oxide quantum dot (GOQDs) has very large difference, when excitation wavelength is 300nm, its highest peak appears at 407nm, there is obvious blue shift in the fluorescence that is relative graphene oxide quantum dot, by blue light (441nm), is blue shifted to purple light (407nm).Having there is obvious variation in the energy band structure of explanation graphene oxide quantum dot at this temperature, illustrates that this annealing temperature is very large on the impact of product component.
Fig. 7 is the fluorescence spectrum result of the sample of example 7 tests, and as seen from the figure, when excitation wavelength is 300nm, the peak position of graphene oxide quantum dot is 441nm(blue light).Annealing temperature is that the fluorescence highest peak of 300 ℃, 600 ℃ and 900 ℃ is respectively at 431nm(blue light), 413nm(purple light) and 407nm(purple light).Result shows the rising along with annealing temperature, and obvious blue shift has appearred in its fluorescence.We can regulate the luminous position of graphene oxide quantum dot by selective annealing temperature, can realize adjustable from blue light to purple light.
Although prior art scheme of the present invention and preferred embodiment statement are as above, so it is not in order to limit the present invention.Persond having ordinary knowledge in the technical field of the present invention, without departing from the spirit and scope of the present invention, when doing various variations, substitute and retouching.Therefore, protection scope of the present invention is when being as the criterion depending on claims person of defining.
Claims (10)
1. a method of preparing purple fluorescence redox graphene quantum dot, is characterized in that comprising the steps:
(1) take graphene oxide as starting material, using nitric acid, sulfuric acid as oxygenant, the ratio that adds 25ml-35ml nitric acid, 5ml-15ml sulfuric acid with every 50mg graphene oxide carries out invading for 20-30 hour bubble oxide treatment to graphene oxide;
(2) the graphene oxide solution after oxidation in step (1) is carried out to 10-18 hour ultrasonic decomposition;
(3) utilize the graphene oxide solution after ultrasonic in deionized water dilution step (2);
(4) the graphene oxide solution after dilution in step (3) is carried out to centrifugal disacidify processing;
(5) the graphene oxide sample after utilizing deionized water to disacidify in step (4) carries out repeatedly eccentric cleaning, until solution ph is adjusted to 8;
(6) gained solution in step (5) is carried out to high-pressure digestion 10-14 hour at 200 ± 20 ℃;
(7) dialysis tubing of the soln using 8000～14000Da after clearing up in step (6) is carried out to the continuous dialysis of 5-10 days;
(8) collect the solution of dialysing outside back pkt. continuously in step (7), under 90 ± 5 ℃ of conditions, carry out drying and processing;
(9) by drying gained graphene oxide quantum dot powder in step (8), pack quartz boat into and put into silica tube, at H
2lower 300 ℃ of-900 ℃ of thermal reduction 40-80 minute of atmosphere, close hydrogen, import at once argon gas, allow silica tube naturally cool to room temperature, obtain redox graphene quantum dot.
2. prepare according to claim 1 the method for purple fluorescence redox graphene quantum dot, it is characterized in that described step (1) take graphene oxide as starting material, using nitric acid, sulfuric acid as oxygenant, and the ratio that adds 30ml nitric acid, 10ml sulfuric acid with every 50mg graphene oxide carries out invading for 24 hours bubble oxide treatment to graphene oxide.
3. prepare according to claim 1 the method for purple fluorescence redox graphene quantum dot, it is characterized in that utilizing in step (2) ultrasonic machine of 200W that the graphene oxide solution after oxidation in step (1) is carried out to 10-18 hour ultrasonic decomposition.
4. prepare according to claim 1 the method for purple fluorescence redox graphene quantum dot, it is characterized in that the graphene oxide solution after ultrasonic in step (2) is that 1-1.5:5 mixes with deionized water described in step (3) according to volume ratio, the graphene oxide solution after ultrasonic in dilution step (2).
5. prepare according to claim 1 the method for purple fluorescence redox graphene quantum dot, it is characterized in that in step (4), utilizing high speed freezing centrifuge to adopt the rotating speed of 10000-18000 rev/min to carry out repeatedly disacidify to the graphene oxide solution after diluting in step (3) processes, each centrifugation time is 30-50 minute.
6. prepare according to claim 1 the method for purple fluorescence redox graphene quantum dot, it is characterized in that in step (4), the graphene oxide sample after disacidify is that 1-1.5:5 mixes with deionized water described in step (5) according to mass ratio, and stir, carry out eccentric cleaning 10-15 time, until solution ph is adjusted to 8.
7. prepare according to claim 1 the method for purple fluorescence redox graphene quantum dot, it is characterized in that, in step (6), gained soln using high-pressure digestion tank in step (5) is carried out to high-pressure digestion 10-14 hour at 200 ± 20 ℃.
8. prepare according to claim 1 the method for purple fluorescence redox graphene quantum dot, it is characterized in that H in described step (9)
2flow be 100sccm-200sccm.
9. prepare according to claim 1 the method for purple fluorescence redox graphene quantum dot, it is characterized in that in silica tube, making H in described step (9)
2remain on a normal atmosphere.
10. prepare according to claim 1 the method for purple fluorescence redox graphene quantum dot, it is characterized in that in described step (8) that 200Pa is with dry under interior pressure.
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Cited By (8)
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| CN104386673A (en) * | 2014-10-29 | 2015-03-04 | 安徽师范大学 | Graphene quantum dots (GQDs) and preparation method thereof |
| CN104650862A (en) * | 2015-01-22 | 2015-05-27 | 南京邮电大学 | Preparation and applications of graphene quantum dots with white fluorescence emission properties |
| CN107431211A (en) * | 2014-11-06 | 2017-12-01 | 威廉马歇莱思大学 | By the method for various carbon sources manufacture graphene quantum dot |
| CN107601466A (en) * | 2017-10-12 | 2018-01-19 | 青岛科技大学 | A kind of preparation method and applications of the graphene quantum dot of size uniform |
| CN107720734A (en) * | 2017-11-20 | 2018-02-23 | 泉州师范学院 | It is a kind of to prepare the method with fluorescent characteristic graphene quantum dot using waste biomass resource |
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| CN104386673A (en) * | 2014-10-29 | 2015-03-04 | 安徽师范大学 | Graphene quantum dots (GQDs) and preparation method thereof |
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| CN107431211A (en) * | 2014-11-06 | 2017-12-01 | 威廉马歇莱思大学 | By the method for various carbon sources manufacture graphene quantum dot |
| CN104650862A (en) * | 2015-01-22 | 2015-05-27 | 南京邮电大学 | Preparation and applications of graphene quantum dots with white fluorescence emission properties |
| CN107601466A (en) * | 2017-10-12 | 2018-01-19 | 青岛科技大学 | A kind of preparation method and applications of the graphene quantum dot of size uniform |
| CN107601466B (en) * | 2017-10-12 | 2018-08-03 | 青岛科技大学 | A kind of preparation method and applications of the graphene quantum dot of size uniform |
| CN107720734A (en) * | 2017-11-20 | 2018-02-23 | 泉州师范学院 | It is a kind of to prepare the method with fluorescent characteristic graphene quantum dot using waste biomass resource |
| CN110194839A (en) * | 2019-06-25 | 2019-09-03 | 西北师范大学 | A kind of preparation and application of graphene quantum dot/polyphenyl thioether composite material |
| WO2022088295A1 (en) * | 2020-10-27 | 2022-05-05 | 华侨大学 | Fluorescent reduced graphene oxide, and preparation method therefor and application thereof |
| 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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