CN114014312B - Preparation method and application of water-soluble efficient luminescent graphene oxide quantum dots - Google Patents
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Abstract
The invention belongs to the field of material preparation, and particularly relates to a preparation method of a water-soluble efficient green luminescent graphene quantum dot and application of the quantum dot in cell imaging. The preparation method comprises the following steps: step 1: preparing graphene oxide; and 2, step: and (3) carrying out ultrasonic treatment on the graphene oxide by using a cell disruption instrument. The graphene oxide quantum dot solid prepared by the preparation method has good water solubility, and the quantum efficiency of the graphene oxide quantum dot dissolved in water can reach 14.9%. In addition, the obtained graphene oxide quantum dots have good cell compatibility and low cytotoxicity, so that the graphene oxide quantum dots can be applied to cell imaging.
Description
Technical Field
The invention belongs to the field of material preparation, and particularly relates to a preparation method of a water-soluble efficient green luminescent graphene quantum dot and application of the quantum dot in cell imaging.
Background
Generally, the particle size of graphene is approximately distributed from tens of nanometers to hundreds of nanometers and occasionally reaches the micron level, when the size of the material is smaller than the exciton bohr radius, the movement of electrons and holes is limited, and the characteristic of quantization is presented, and such a nano structure is called a quantum dot. The graphene quantum dots have sp2 and sp3 hybridized carbon structures, generally have single-layer or multi-layer graphite structures, and when two-dimensional graphene micro-sheets are crushed to a nano-scale, graphene shows the characteristics of a semiconductor. The carbon-based quantum dots with the grain diameter of about 10nm or even less than 10nm have a plurality of unique properties due to quantum surface effect, confinement effect, quantum size effect, macroscopic quantum effect and small size effect; the luminous efficiency is enhanced, the luminous peak position is regulated and controlled by the size, and the multi-exciton effect is realized. Graphene quantum dots have many advantages: 1. the biocompatibility is good; 2. low cytotoxicity; 3. the raw materials are easy to obtain; 4. has a light emitting property; 5. good electrical properties; 6. chemical inertness, and the like.
In recent years, people have made certain progress in the synthesis research of graphene quantum dots, and various synthesis methods have been developed successively. Most synthesis methods use graphite, graphene oxide, activated carbon, carbon nanotubes, carbon fibers and the like as precursors, and the precursors are crushed by physical, chemical and electrochemical methods to obtain graphene luminescent quantum dots. Although various methods for preparing graphene oxide luminescent quantum dots exist, there are certain problems, such as: low synthesis efficiency and fluorescence efficiency, the fluorescence emission wavelength is mostly in a blue light region, and the light-emitting spectrum has a dependency relationship with the excitation wavelength. For example, researchers have a method for preparing graphene quantum dots by oxidizing graphite at high temperature with potassium permanganate, concentrated sulfuric acid and sodium nitrate, but the fluorescence quantum efficiency of the graphene quantum dots obtained by the method is very low and is less than 1%. For another example, researchers have broken graphene oxide in DMF solution at high temperature to obtain graphene quantum dots with fluorescence quantum efficiency of over 10%, but the reaction conversion rate of this synthesis method is only 1.6%. Generally, the light-emitting efficiency of most of the graphene quantum dots obtained by the method is generally low, and particularly, the water-soluble efficient light-emitting graphene quantum dots are not obtained, so that the application of the graphene quantum dots in the fields of biomedical imaging, LED display and the like is influenced, and a simple and effective preparation method is urgently needed to be developed.
It is still a great challenge to develop a simple, fast, convenient and environment-friendly method for obtaining graphene quantum dots with high quantum yield.
Disclosure of Invention
In order to overcome the problem that the quantum efficiency of the graphene quantum dots prepared by the existing method is insufficient, the invention provides the preparation method which is used for preparing the graphene oxide by the improved hummer method, greatly improving the quantum efficiency of the graphene quantum dots and the conversion rate of the graphene oxide by utilizing the tip ultrasonic technology, obtaining the high-efficiency green luminescent graphene quantum dots, and applying the high-efficiency green luminescent graphene quantum dots to biological imaging.
The invention specifically adopts the following technical scheme:
a preparation method of water-soluble efficient green luminescent graphene quantum dots comprises the following steps:
step 1: preparing graphene oxide:
(1) Graphene oxide was prepared by a modified Hummer method. The preparation method comprises the steps of firstly carrying out ice bath on concentrated sulfuric acid in a flask for a period of time, and then adding graphene nanoplatelets into the concentrated sulfuric acid to fully expand the graphene.
Specifically, the concentrated sulfuric acid is 98% concentrated sulfuric acid by mass, the ice-bath time is 15min, and the ratio of graphene to concentrated sulfuric acid is 20 (mg/mL).
(2) Stirring in ice bath, slowly adding potassium permanganate, and changing the solution from transparent to dark green. The reaction was kept stirring for 12h at 35 ℃ until the solution became an earthy yellow viscous slurry.
Specifically, the stirring time under ice bath is 30min, and the mass ratio of potassium permanganate to graphene is 4.
(3) The water bath is removed, ultrapure water is added in portions, and then stirring reaction is continued at 35 ℃ for 2h.
Specifically, the ultrapure water is because concentrated sulfuric acid dilution can release heat, the temperature is prevented from being too high, and the amount of ultrapure water added each time is just good, so that the khaki viscous slurry can be well dispersed in water.
(4) Adding hydrogen peroxide with the mass percent of 30%, and stirring until the solution turns golden yellow.
The hydrogen peroxide has strong oxidizing property, the solution turns golden yellow after being added, and the adding amount of the hydrogen peroxide just leads the solution to turn golden yellow, so that the color cannot be darker when more solutions are added.
(5) And (5) washing. Adding hydrochloric acid into the golden yellow solution prepared in the step (4) at the rotating speed of 10000rpm/min for washing; then, distilled water was added to the above solution at 10000rpm/min for washing. Discarding the upper layer turbid liquid, and taking the lower layer precipitate to obtain the graphene oxide.
Specifically, the hydrochloric acid is obtained by mixing 36-38% of concentrated hydrochloric acid in mass fraction with water according to a volume ratio of 1.
And 2, step: carrying out ultrasonic treatment on graphene oxide by using a cell disruptor:
(1) And (2) freeze-drying the graphene oxide precipitate prepared in the step 1 for 12 hours to obtain a dried graphene oxide solid, and adding N, N-dimethylformamide into the graphene oxide solid to form a graphene oxide suspension liquid with the mass concentration of 10mg/mL.
(2) Carrying out ultrasonic treatment on the graphene oxide turbid liquid for 10min by using a cell disruptor, stirring the graphene oxide turbid liquid, transferring the graphene oxide turbid liquid into 100mL of polytetrafluoroethylene in a reaction kettle, controlling the filling rate of the reaction kettle to be 80%, putting the mixture into a drying oven, heating the mixture for 12h at 200 ℃, naturally cooling the mixture to room temperature after the reaction is finished, and filtering the mixture by using a microporous filter head to obtain a graphene oxide quantum dot solution in DMF.
Wherein, the ultrasonic mode of the cell crusher is that the ultrasonic is switched on for 3s and switched off for 5s, the power ratio is 6 percent, and the power is 900W.
In addition, before the cell disruption instrument is used for ultrasonic treatment, an ultrasonic cleaner is used for ultrasonic treatment for 30min, and the ultrasonic power of an ultrasonic machine is 600W.
(3) And (3) putting the graphene oxide quantum dot solution in the DMF into a rotary evaporator for processing to obtain a dry graphene oxide quantum dot solid.
The prepared graphene oxide quantum dot solid can emit green fluorescence under different excitation wavelengths such as 380-480 nm and has low cytotoxicity, so that the graphene oxide quantum dot solid can be applied to cell imaging.
The beneficial effects of the invention are as follows:
the graphene oxide quantum dot solid prepared by the preparation method has good water solubility, and the quantum efficiency of the graphene oxide quantum dot dissolved in water can reach 14.9%. In addition, the obtained graphene oxide quantum dots have good cell compatibility and low cytotoxicity, so that the graphene oxide quantum dots can be applied to cell imaging.
Drawings
Fig. 1 is an absorption diagram of a graphene oxide dispersion liquid prepared in an embodiment of the present invention.
Fig. 2 is an AFM image of the graphene oxide prepared in the example of the present invention.
Fig. 3 is a fluorescence diagram of efficient green luminescent graphene quantum dots prepared from different concentrations (mg/mL) of graphene oxide DMF suspensions prepared in the embodiment of the present invention and different filling degrees (%) of the graphene oxide suspensions in a reaction kettle.
Fig. 4 is a fluorescence diagram of the high-efficiency green-luminescent graphene quantum dots in water by using tip ultrasound at different times, which is prepared in the embodiment of the invention.
Fig. 5 shows an absorption spectrum, an excitation spectrum, and a fluorescence spectrum of the high-efficiency green luminescent graphene quantum dot prepared in the embodiment of the present invention.
Fig. 6 shows the particle size distribution of the high-efficiency green luminescent graphene quantum dots prepared in the embodiment of the present invention.
Fig. 7 is an AFM image of the high-efficiency green luminescent graphene quantum dot prepared in the embodiment of the present invention.
Fig. 8 is a fluorescence diagram of the efficient green-emitting graphene quantum dots prepared in the embodiment of the present invention under different excitation wavelengths.
Fig. 9 is a cytotoxicity detection diagram of the high-efficiency green luminescent graphene quantum dot prepared in the embodiment of the invention.
Fig. 10 is an imaging merge image of the efficient green-emitting graphene quantum dots prepared in the embodiment of the present invention in hela cells under 488nm excitation light.
Detailed Description
The present invention will be described in more detail with reference to the following embodiments, which are provided for understanding the technical solutions of the present invention, but are not intended to limit the scope of the present invention.
Example 1
1. Preparing graphene oxide:
(1) Graphene oxide was prepared by a modified Hummer method. Specifically, 25mL of concentrated sulfuric acid with the mass concentration of 98% is firstly subjected to ice bath in a flask for 15min, and ice blocks are continuously added in the ice bath process. And adding 500mg of graphene nanoplatelets into concentrated sulfuric acid to fully expand the graphene.
(2) Stirring is carried out for 30min under ice bath, and 2g of potassium permanganate is slowly added, at which time the solution changes from transparent to dark green. The reaction was kept at 35 ℃ with stirring for 12h until the solution became an earthy yellow viscous slurry.
(3) The water bath was removed and 12mL of ultrapure water was added in six portions, after which the reaction was continued at 35 ℃ for 2h.
(4) Adding 7.5mL of 30% hydrogen peroxide by mass, and stirring for 15min to obtain a golden yellow solution.
(5) And (5) washing. Mixing concentrated hydrochloric acid with the mass fraction of 36-38% with water according to the volume ratio of 1. Adding the diluted hydrochloric acid into the golden yellow solution prepared in the step (4) at the rotating speed of 10000rpm/min for washing, wherein five minutes and three times are carried out for washing each time; distilled water was further added to the above solution at 10000rpm/min for washing for 20 minutes each time, and the washing was carried out three times. The upper suspension is discarded, the absorption diagram of the upper suspension is shown in fig. 1, and fig. 1 shows that graphene oxide (a small amount of graphene exists in the suspension) is prepared, the absorption peak at 229nm comes from pi-pi transition of a C = C double bond, and the absorption peak at 300nm comes from n-pi transition of a C = O double bond. And (3) precipitating the lower layer to obtain graphene oxide, wherein an AFM (atomic force microscopy) diagram of the obtained graphene oxide is shown in FIG. 2, and FIG. 2 illustrates that the prepared graphene oxide is of a single-layer structure and has relatively good purity.
2. Performing tip ultrasound on graphene oxide by using a cell disruptor:
freezing the graphene oxide precipitate obtained in the first step at-22 ℃ by using a refrigerator, then placing the graphene oxide precipitate into a freeze drying oven at-56 ℃ for 12 hours to obtain a dried graphene oxide solid (GO), and adding N, N-Dimethylformamide (DMF) into the graphene oxide solid to respectively form graphene oxide turbid liquids with mass concentrations of 0.5mg/mL, 1mg/mL, 5mg/mL, 10mg/mL and 20 mg/mL. And pouring the graphene oxide suspension into a beaker, putting the graphene oxide suspension into an ultrasonic cleaner (Beijing Tian you Hengda science and technology Co., ltd., model: TYHD-600, power: 600 w), performing medium-ultrasonic treatment for half an hour, cooling the suspension, and further performing tip ultrasonic treatment by putting an ultrasonic cell disruption instrument (Ningbo Xinzhi Biotechnology Co., ltd., model: LC-JY92-IIN, ultrasonic power: 900 w) in an ultrasonic mode of turning on and off the ultrasonic cell disruption instrument for 3s and 5s, wherein the power ratio is 6%. Respectively processing the materials in an ultrasonic cell disruption instrument for 0min, 5min, 10min, 15min, 20min and 25min, stirring the graphene oxide suspension, transferring the graphene oxide suspension into 100mL of polytetrafluoroethylene, controlling the filling rates to be 100%, 80%, 60% and 40%, respectively, putting the mixture into an oven, heating the mixture at 200 ℃ for 12h, naturally cooling the mixture to room temperature after the reaction is finished, and filtering the mixture by using a 220nm microporous filter head to obtain the graphene oxide quantum dot solution in DMF. The redundant graphene oxide solid in the solution is firstly centrifuged before the filter head is used for filtering, because partial graphene oxide can not be cracked into graphene quantum dots during reaction in a reaction kettle, and the graphene quantum dots are all dissolved in the DMF solution, the graphene oxide solid is separated out by centrifugation, and then large particles are filtered by the 220nm filter head, so that pure graphene quantum dots can be obtained.
The mass concentration (mg/mL) of the graphene oxide DMF suspension and the degree of filling of the graphene oxide DMF suspension in the reaction kettle (100%, 80%, 60%, 40%) have the influence on the fluorescence of the graphene oxide quantum dots as shown in fig. 3. Fig. 3A shows: graphene oxide with different masses (mg) is dissolved in DMF with different volumes (mL), so that the fluorescence patterns of the graphene quantum dots are different in height, and a proper proportion, namely the quantum dots have the strongest fluorescence when GO/DMF is 10mg/mL, is obtained through screening. Fig. 3B shows: the filling rate percentage is the degree of the polytetrafluoroethylene container solution in the reaction kettle, 100% represents full, and the quantum dot has the strongest fluorescence when the filling rate is 80% through screening.
Putting the graphene oxide quantum dot solution in DMF (dimethyl formamide) into a rotary evaporator for 0.5 hour, controlling the temperature to be 55 ℃, obtaining dry graphene oxide quantum dot solid, and then adding ultrapure water into the dry graphene oxide quantum dot solid to obtain the graphene oxide quantum dot solution in water.
The fluorescence profiles of the graphene oxide quantum dots in water obtained at different sonication cell disruption instrument treatment times are shown in fig. 4. Fig. 4 shows that different ultrasonic times have an effect on the fluorescence of the graphene quantum dots in water, and the ultrasonic time of 10 minutes is the best, and the fluorescence of the quantum dots in water is the highest.
The absorption spectrum, excitation spectrum, fluorescence spectrum, particle size and morphology of the graphene oxide quantum dots are respectively shown in fig. 5, 6 and 7. FIG. 5 illustrates the best excitation wavelength of 380nm of quantum dots, the fluorescence peak position under 380nm excitation is near 500nm, and the upper right corner of FIG. 5 is a real image under ultraviolet lamp irradiation. FIGS. 6 and 7 show that the average particle size of the quantum dots is about 6.3nm and the height is uniform. Fig. 8 shows that the light-emitting position of the quantum dot can be slightly shifted and has slight wavelength dependence under different excitation wavelengths.
3. Application of efficient green luminescent graphene oxide quantum dots
Toxicity measurements were performed on hela cells using high efficiency green emitting graphene quantum dots at different concentrations (0 μ g, 25 μ g, 50 μ g, 100 μ g, 200 μ g).
500mL Heila cell culture: 445mL of bovine serum albumin and then 5mL of antibiotic were added to 445mL of MEM.
Firstly, seeding HeLa cells on a 96-well plate, setting a blank control, five multiple wells, five concentration gradients (0 mug, 25 mug, 50 mug, 100 mug and 200 mug) and 5 multiple wells, adding samples GQDs with different concentrations into the five multiple wells, incubating for 12 hours, measuring the cell survival rate every three hours to obtain an average value, and obtaining a result shown in figure 9, wherein figure 9 shows that the graphene quantum dots have low toxicity and can be applied to cell imaging.
The cell climbing sheet is manufactured, graphene oxide quantum dots are led into a Hela cell, a confocal microscope is used for cell imaging under 488nm laser, merge images in the Hela cell are shown in figure 10, and the result shows that the graphene quantum dots can well enter the Hela cell, green fluorescence is emitted under 488nm laser, and the graphene oxide quantum dots can be applied to cell imaging.
The above-described embodiments are merely preferred embodiments of the present invention, and not intended to limit the scope of the invention, so that equivalent changes or modifications in the structure, features and principles described in the present invention should be included in the claims of the present invention.
Claims (9)
1. A preparation method of water-soluble efficient green luminescent graphene quantum dots is characterized by comprising the following steps:
step 1: preparing graphene oxide:
1.1: carrying out ice bath on concentrated sulfuric acid, and then adding the graphene nanoplatelets into the concentrated sulfuric acid to expand the graphene;
1.2: stirring in ice bath, adding potassium permanganate, keeping the solution at 35 ℃ for continuous stirring reaction until the solution becomes yellowish-brown thick slurry;
1.3: removing the water bath, adding ultrapure water for several times, and then continuing stirring at 35 ℃ for reaction for 2 hours;
1.4: adding hydrogen peroxide with the mass percent of 30%, and stirring until the solution turns golden yellow;
1.5: washing: adding hydrochloric acid into the golden yellow solution prepared in the step 1.4 for washing; then adding distilled water into the solution for washing; discarding the upper layer turbid liquid, and taking the lower layer precipitate to obtain graphene oxide;
and 2, step: carrying out ultrasonic treatment on graphene oxide by using a cell disruptor:
2.1: freeze-drying the graphene oxide precipitate prepared in the step 1 to obtain a dried graphene oxide solid, and adding DMF (dimethyl formamide) into the graphene oxide solid to form a graphene oxide suspension;
2.2: carrying out ultrasonic treatment on the graphene oxide suspension by using a cell disruption instrument, stirring the graphene oxide suspension, transferring the graphene oxide suspension into a polytetrafluoroethylene reaction kettle, heating the graphene oxide suspension in an oven at 200 ℃ for 12 hours, naturally cooling the graphene oxide suspension to room temperature after the reaction is finished, and filtering the mixture to obtain a graphene oxide quantum dot solution in DMF (dimethyl formamide);
2.3: and (3) putting the graphene oxide quantum dot solution in the DMF into a rotary evaporator for processing to obtain a dry graphene oxide quantum dot solid.
2. The method for preparing the water-soluble efficient green luminescent graphene quantum dot according to claim 1, wherein in step 1.1, the concentrated sulfuric acid is 98% concentrated sulfuric acid, and the ratio of the graphene to the concentrated sulfuric acid is 20mg.
3. The preparation method of the water-soluble efficient green luminescent graphene quantum dot according to claim 1, characterized in that in step 1.1, stirring is carried out for 30min under ice bath, and the mass ratio of potassium permanganate to graphene is 4.
4. The method for preparing the water-soluble efficient green luminescent graphene quantum dot according to claim 1, wherein in the step 1.3, the amount of ultrapure water is added each time so that the khaki viscous slurry can be dispersed in water.
5. The preparation method of the water-soluble efficient green luminescent graphene quantum dot according to claim 1, wherein in step 1.5, the hydrochloric acid is obtained by mixing 36-38% mass fraction concentrated hydrochloric acid and water according to a volume ratio of 1.
6. The method for preparing the water-soluble efficient green luminescent graphene quantum dot according to claim 1, wherein in the step 2.1, the concentration of the graphene oxide suspension is 10mg/mL.
7. The preparation method of the water-soluble efficient green luminescent graphene quantum dot according to claim 1, wherein in the step 2.2, the filling rate of a polytetrafluoroethylene reaction kettle is 80%.
8. The preparation method of the water-soluble efficient green luminescent graphene quantum dot according to claim 1, wherein in the step 2.2, before the cell disruption instrument is used for ultrasonic treatment, an ultrasonic cleaner is used for ultrasonic treatment for 30min, and the ultrasonic machine has an ultrasonic power of 600W; the ultrasonic mode of the cell crusher is that the ultrasonic is switched on for 3s and off for 5s, the power ratio is 6 percent, the power is 900W, and the ultrasonic time of the cell crusher is 10min.
9. The application of the graphene oxide quantum dot solid prepared by the preparation method of any one of claims 1 to 8 in cell imaging.
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