CN104449693A - Method for preparing nitrogen and sulfur-doped fluorescent carbon quantum dots - Google Patents
Method for preparing nitrogen and sulfur-doped fluorescent carbon quantum dots Download PDFInfo
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Abstract
The invention discloses a method for preparing nitrogen and sulfur-doped fluorescent carbon quantum dots. According to the method, citric acid is taken as a carbon source, L-glutathione is taken as a nitrogen-sulfur dopant, a microwave oven is taken as a reaction platform, the carbon quantum dots with fluorescence properties are prepared in a heating manner, the residues and moisture are removed through dialysis and freeze drying, and quantum dot powder is obtained. The nitrogen and sulfur-doped carbon quantum dots are prepared by adopting the method disclosed by the invention; the method is simple in operation, low in cost, high in yield, simple in preparation process and equipment, free of a solvent, and easy to popularize and produce on a large scale, and can be rapidly finished within a short period of time; and the prepared carbon quantum dots have the advantages of good water solubility, high fluorescence properties, photobleaching resistance, adjustable emission spectrum, good biocompatibility, low cytotoxicity and the like, and have a good application prospect in the fields of bioimaging, biosensors and photo-electric devices.
Description
Technical field
The present invention relates to technical field of nano material, be specifically related to a kind of preparation method of fluorescent carbon quantum dot of nitrogen sulfur doping.
Background technology
In recent years, carbon quantum dot (Carbon dots, particle diameter < 10 nm) causes showing great attention to of investigator as a kind of novel zero-dimension nano fluorescent material.Compare with traditional heavy metal semiconductor-quantum-point with organic dye, carbon quantum dot owing to having extensive chemical inertia, high stability, low cytotoxicity, good biocompatibility and the feature such as water-soluble, and make that it can be potential for sensor, photochemical catalysis, bio-imaging and area of solar cell.
Up to now, a lot of method such as laser lift-off Graphene, electrochemical oxidation process, arc discharge method, solvent hydrothermal method, chemical oxidization method and high temperature pyrolytic cracking (HTP) etc. have been used to the preparation of carbon quantum dot, but, these methods major part building-up processes are loaded down with trivial details, expensive starting materials and condition is harsh etc., these methods are uneconomical environmental protection not only, and too high owing to synthesizing cost, greatly limit scale operation and the practical application of fluorescent carbon quantum dot.Therefore, explore a kind of simple, quick, that the preparation of low cost, nontoxic and eco-friendly green method has high fluorescence property carbon quantum dot to have great importance.
Summary of the invention
The object of the invention is the deficiency existed for prior art, a kind of method can being prepared the fluorescent carbon quantum dot of nitrogen sulfur doping by solid phase microwave-assisted is provided, and the application of this carbon quantum dot.
Technical scheme of the present invention provides a kind of method of fluorescent carbon quantum dot of nitrogen sulfur doping, it is characterized in that, comprises the following steps:
(1) citric acid and nitrogen sulfur doping agent powder are put into agate mortar to grind, obtain uniform white powder;
(2) above-mentioned white powder is put into microwave oven, adopt 700 W power, microwave radiation 1.5 ~ 3 min, obtain carbon quantum dot solid;
(3) solid obtained in (2) is dissolved in 5 mL water, ultrasonicly obtain uniform carbon quantum dot solution;
(4) be injected in dialysis tubing by the solution obtained in step (3) and dialyse, its molecular weight cut-off is 500 D, and dialysis time is 48 h, changes a water at interval of 6 h;
(5) dialysis product is evaporated, obtain concentrated solution;
(6) by carrying out lyophilize under concentrated solution – 50 DEG C of conditions to Powdered, the carbon quantum dot of nitrogen sulfur doping is obtained.
The agent of described nitrogen sulfur doping is L – gsh.
In described step (1), citric acid powder gets 0.6 g, and 0.2 g is got in the agent of nitrogen sulfur doping.
Advantage of the present invention:
(1) the present invention is simple to operate, and without the need to any solvent, and do not need complicated follow-up process, single stage method can obtain carbon quantum dot.
(2) preparation technology's equipment is simple, only needs domestic microwave oven to complete, does not have the particular requirements such as protective atmosphere, vacuum tightness and high temperature, and in several minutes, get final product complete operation, is easy to promote and scale operation.
(3) carbon quantum dot of the nitrogen sulfur doping obtained, soluble in water, fluorescence quantum yield improves greatly, good light stability, and cytotoxicity is low, has a good application prospect.
Accompanying drawing explanation
The photo of the carbon quantum dot aqueous solution under 365 nm UV-irradiation that Fig. 1 is embodiment one (a), embodiment two (b), embodiment three (c) are prepared with embodiment four (d).
Fig. 2 is the fluorogram of the carbon quantum dot aqueous solution under 360 nm excite of embodiment one, embodiment two, embodiment three and embodiment four times preparations.
Fig. 3 is the fluorescence emission spectrogram of the carbon quantum dot aqueous solution under different excitation wavelength prepared by embodiment three.
Fig. 4 is the transmission electron microscope picture of carbon quantum dot prepared by embodiment three.
Fig. 5 be embodiment three prepare carbon quantum dot under different concns to the cytotoxicity figure of HeLa cell.
embodiment:
Below by way of specific embodiment, technical solution of the present invention is described.
Embodiment one:
(1) citric acid 0.6 g and L – gsh powder 0.2 g is put into agate mortar to grind, obtain uniform white powder;
(2) above-mentioned white powder is put into microwave oven, adopt 700 W power, microwave radiation 1.5 min, obtain white carbon quantum dot solid;
(3) white solid obtained in (2) is dissolved in 5 mL water, ultrasonicly obtain uniform carbon quantum dot solution;
(4) be injected in dialysis tubing by the solution obtained in step (3) and dialyse, its molecular weight cut-off is 500 D, and dialysis time is 48 h, changes a water at interval of 6 h;
(5) dialysis product is evaporated, obtain concentrated solution;
(6) by carrying out lyophilize under concentrated solution – 50 DEG C of conditions to Powdered, the carbon quantum dot of nitrogen sulfur doping is obtained, yield about 2%, quantum yield about 4.5%.
Embodiment two:
(1) citric acid 0.6 g and L – gsh powder 0.2 g is put into agate mortar to grind, obtain uniform white powder;
(2) above-mentioned white powder is put into microwave oven, adopt 700 W power, microwave radiation 2 min, obtain brown carbon quantum dot solid;
(3) brown solid obtained in (2) is dissolved in 5 mL water, ultrasonicly obtain uniform carbon quantum dot solution;
(4) be injected in dialysis tubing by the solution obtained in step (3) and dialyse, its molecular weight cut-off is 500 D, and dialysis time is 48 h, changes a water at interval of 6 h;
(5) dialysis product is evaporated, obtain concentrated solution;
(6) by carrying out lyophilize under concentrated solution – 50 DEG C of conditions to Powdered, the carbon quantum dot of nitrogen sulfur doping is obtained, yield about 12%, quantum yield about 50%.
Embodiment three:
(1) citric acid 0.6 g and L – gsh powder 0.2 g is put into agate mortar to grind, obtain uniform white powder;
(2) above-mentioned white powder is put into microwave oven, adopt 700 W power, microwave radiation 2.5 min, obtain reddish-brown carbon quantum dot solid;
(3) red brown solid obtained in (2) is dissolved in 5 mL water, ultrasonicly obtain uniform carbon quantum dot solution;
(4) be injected in dialysis tubing by the solution obtained in step (3) and dialyse, its molecular weight cut-off is 500 D, and dialysis time is 48 h, changes a water at interval of 6 h;
(5) dialysis product is evaporated, obtain concentrated solution;
(6) by carrying out lyophilize under concentrated solution – 50 DEG C of conditions to Powdered, the carbon quantum dot of nitrogen sulfur doping is obtained, yield about 15%, quantum yield about 68%.
Embodiment four:
(1) citric acid 0.6 g and L – gsh powder 0.2 g is put into agate mortar to grind, obtain uniform white powder;
(2) above-mentioned white powder is put into microwave oven, adopt 700 W power, microwave radiation 3 min, obtain reddish-brown carbon quantum dot solid;
(3) red brown solid obtained in (2) is dissolved in 5 mL water, ultrasonicly obtain uniform carbon quantum dot solution;
(4) be injected in dialysis tubing by the solution obtained in step (3) and dialyse, its molecular weight cut-off is 500 D, and dialysis time is 48 h, changes a water at interval of 6 h;
(5) dialysis product is evaporated, obtain concentrated solution;
(6) by carrying out lyophilize under concentrated solution – 50 DEG C of conditions to Powdered, the carbon quantum dot of nitrogen sulfur doping is obtained, yield about 16.5%, quantum yield about 60%.
Embodiment sample is characterized
The UV-light of 365 nm is utilized to irradiate the carbon quantum dot aqueous solution prepared by embodiment, can be observed that a is blue (embodiment one), b is blue-greenish colour (embodiment two), c be blue-greenish colour (embodiment three) and d is blue-greenish colour (embodiment four), see Fig. 1.
The fluorescence emission spectrum of the carbon quantum dot aqueous solution under 360 nm excite utilizing fluorescence visible spectrophotometer sign embodiment one (a), embodiment two (b), embodiment three (c) and embodiment four (d) to prepare characterizes, see Fig. 2.
Utilize fluorescence visible spectrophotometer to investigate excitation wavelength to the impact of carbon quantum dot aqueous solution fluorescence prepared by embodiment three, see Fig. 3.
Transmission electron microscope is utilized to characterize the pattern of carbon quantum dot.Result shows, the carbon quantum dot of preparation is about 2 nm, rotund and single dispersion, sees Fig. 4.
After HeLa cell and the carbon quantum dot nutrient solution containing different concns are hatched 24 h, utilize the motility rate of mtt assay to HeLa cell to investigate, see Fig. 5.
Claims (4)
1. a preparation method for the fluorescent carbon quantum dot of nitrogen sulfur doping, is characterized in that, comprises the following steps:
(1) citric acid and nitrogen sulfur doping agent powder are put into agate mortar to grind, obtain uniform white powder;
(2) above-mentioned white powder is put into microwave oven, adopt 700 W power, microwave radiation 1.5 ~ 3 min, obtain carbon quantum dot solid;
(3) solid obtained in step (2) is dissolved in 5 mL water, ultrasonicly obtain uniform carbon quantum dot solution;
(4) be injected in dialysis tubing by the solution obtained in step (3) and dialyse, its molecular weight cut-off is 500 D, and dialysis time is 48 h, changes a water at interval of 6 h;
(5) dialysis product is evaporated, obtain concentrated solution;
(6) by carrying out lyophilize under concentrated solution – 50 DEG C of conditions to Powdered, the carbon quantum dot of nitrogen sulfur doping is obtained.
2. the preparation method of the fluorescent carbon quantum dot of a kind of nitrogen sulfur doping according to claim 1, is characterized in that: the agent of described nitrogen sulfur doping is L – gsh.
3. the preparation method of the fluorescent carbon quantum dot of a kind of nitrogen sulfur doping according to claim 1, is characterized in that: citric acid powder gets 0.6 g, and 0.2 g is got in the agent of nitrogen sulfur doping.
4. the preparation method of the fluorescent carbon quantum dot of a kind of nitrogen sulfur doping according to claim 1, is characterized in that: the carbon quantum dot of described nitrogen sulfur doping is used for viable cell imaging.
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| CN104804734A (en) * | 2015-04-01 | 2015-07-29 | 河南师范大学 | Synthesis method for sulfur-nitrogen-doped fluorescent carbon dots according to one-step microwave method |
| CN104830328A (en) * | 2015-05-12 | 2015-08-12 | 太原理工大学 | Preparation method of single-matrix carbon quantum dot white light fluorescent powder |
| CN104830326A (en) * | 2015-05-06 | 2015-08-12 | 长江师范学院 | Preparation method of sulfur doped carbon nano dot |
| CN104909349A (en) * | 2015-05-27 | 2015-09-16 | 南昌大学 | Nitrogen-doped fluorescent carbon dot preparation method |
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