CN104927845A - Color-tunable fluorescence carbon dot, and preparation method and application thereof - Google Patents
Color-tunable fluorescence carbon dot, and preparation method and application thereof Download PDFInfo
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- CN104927845A CN104927845A CN201510312058.4A CN201510312058A CN104927845A CN 104927845 A CN104927845 A CN 104927845A CN 201510312058 A CN201510312058 A CN 201510312058A CN 104927845 A CN104927845 A CN 104927845A
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Abstract
The invention discloses a color- tunable fluorescence carbon dot, and a preparation method and application thereof, and belongs to the field of nanometer material science. Leeks are used as a carbon source to prepare a blue fluorescence carbon dot and a green fluorescence carbon dot through a high-temperature pyrolysis method and a hydrothermal method. The raw material of the color-adjustable fluorescence carbon dot is environmentally friendly, the preparation method is simple, and the cost is low; the prepared carbon dot is high in water solubility and stability, and can be used for biolabeling, fluorescence pattern manufacture, fluorescence staining and the like.
Description
Technical field
The present invention relates to the preparation of fluorescent nano material, be specifically related to the preparation method of Color tunable fluorescent carbon point, and the application of the Color tunable fluorescent carbon point of preparation in cell imaging, phosphor pattern making and fluorescent dye.
Background technology
Prepare Color tunable fluorescent carbon point extremely important for the application of carbon point in photodiode and bio-imaging.But the research of this respect is less at present.Document (Microwave-Assisted Synthesis of Wavelength-TunablePhotoluminescent Carbon Nanodots and Their Potential Applications.Hongying Liu, Zhimei He, Liping Jiang, and Junjie Zhu.ACS Appl.Mater.Interfaces, 2015,7,4913-4920), utilize glutaraldehyde and poly-(ethyleneimine) to be carbon source, prepared the fluorescent carbon point of the different wave length of 464-556nm by microwave method.Document (Photoluminescence-Tunable Carbon Nanodots:Surface-State Energy-Gap Tuning.Lei Bao, CuiLiu, Zhiling Zhang, and Daiwen Pang.Adv.Mater., 2015,27,1663 – 1667), utilize nitric acid oxidation carbon fiber, then obtained the fluorescent carbon point of 430 – 610nm different wave lengths by the component of ultrafiltration collection different molecular weight.Document (Color-Switchable, Emission-Enhanced Fluorescence Realized by Engineering C-dotC-dotNanoparticles.Zhen Guo, Zhiqiang Zhang, Wei Zhang, Lianqun Zhou, Haiwen Li, Hongmei Wang, Caroline Andreazza-Vignolle, Pascal Andreazza, Dongxu Zhao, Yihui Wu, Quanlong Wang, TaoZhang, and Keming Jian.ACS Appl.Mater.Interfaces 2014, 6, 20700-20708), utilize citric acid and urea (mass ratio is 1:1) and glycerine and 4 respectively, 7, 10-tri-oxygen-1, 13-tridecane diamine has prepared two kinds of carbon points by hydrothermal method, then this two kinds of carbon points are assembled, define to excite at 455nm and launch yellow respectively down, the carbon point of grass green and golden fluorescence.These methods require loaded down with trivial details synthesis technique or use poisonous/expensive solvent and starting material.
Therefore, the preparation method of research environment-friendly and green, simple Color tunable fluorescent carbon point, has important meaning for the application of fluorescent nano material in bio-imaging, fluorescent printing, sensing etc.
Summary of the invention
The object of the invention is to the defect existed for prior art, a kind of method preparing Color tunable fluorescent carbon point is provided.
Another object of the present invention is to prepared Color tunable fluorescent carbon point to be applied to cell imaging, phosphor pattern makes and fluorescent dye.
For achieving the above object, a kind of method preparing Color tunable fluorescent carbon point provided by the invention take leek as carbon source, by high temperature pyrolytic cracking (HTP) and hydrothermal method obtained blue and green fluorescence carbon point respectively.
Further, a kind of method preparing blue-fluorescence carbon point provided by the invention, comprises the steps:
(1) leek powder metallurgy is carbonized;
(2) product that (1) obtains is mixed with water, obtain dark turbidity liquid;
(3) by dark turbidity liquid through centrifugal, dialysis, finally obtain blue-fluorescence carbon point solution.
The temperature of the described leek high temperature carbonization of step (1) is 250 ~ 350 DEG C, continues 2 ~ 4h.
Centrifugal described in step (3) is with the centrifugal 10min of 4000r/min rotating speed, and described dialysis is the dialysis tubing dialysis 48h of 500 ~ 1000Da with molecular weight cut-off.
A kind of method preparing green fluorescence carbon point provided by the invention, comprises the steps:
(1) leek powder is added in deionized water, obtained mixed solution;
(2) mixed solution that (1) obtains is transferred in hydrothermal reaction kettle, carry out hydro-thermal reaction;
(3) product (2) obtained, through centrifugal, dialysis, finally obtains green fluorescence carbon point solution.
Leek powder described in step (1) mixes 1:10 ~ 100 in mass ratio with deionized water.
The temperature of the hydro-thermal reaction described in step (2) is 200 ~ 300 DEG C, continues 2 ~ 4h.
Centrifugal described in step (3) is with the centrifugal 10min of 4000r/min rotating speed, and described dialysis is the dialysis tubing dialysis 48h of 500 ~ 1000Da with molecular weight cut-off.
The fluorescent carbon point of preparation can make and application in fluorescent dye at cell imaging, phosphor pattern.
The invention has the advantages that:
(1) be carbon source with leek, raw material is extensively easy to get, environmental protection, and preparation method is simple, with low cost;
(2) obtained Color tunable fluorescent carbon point stability is strong, toxic side effect is little, good water solubility, has broad application prospects in fields such as bio-imaging, fluorescent printing, sensings.
Accompanying drawing explanation
Fig. 1 is the fluorescence spectrum figure under the ultraviolet-visible absorption spectroscopy of blue-fluorescence carbon point prepared of embodiment 1 and different wave length optical excitation;
Fig. 2 is the transmission electron microscope picture of blue-fluorescence carbon point prepared by embodiment 2;
Fig. 3 is the infrared spectrogram of blue-fluorescence carbon point prepared by embodiment 3;
Fig. 4 is the fluorescence spectrum figure under the ultraviolet-visible absorption spectroscopy of green fluorescence carbon point prepared of embodiment 4 and different wave length optical excitation;
Fig. 5 is the transmission electron microscope picture of green fluorescence carbon point prepared by embodiment 5;
Fig. 6 is the infrared spectrogram of green fluorescence carbon point prepared by embodiment 6;
Fig. 7 is the cell imaging figure that embodiment 1 and embodiment 4 prepare carbon point;
Fig. 8 is the phosphor pattern construction drawing that embodiment 2 and embodiment 5 prepare carbon point;
Fig. 9 is the fluorescent dye figure that embodiment 3 and embodiment 6 prepare carbon point.
Embodiment
Following examples set forth content of the present invention further, but the present invention is not limited to these embodiments.
Embodiment 1
The preparation of blue-fluorescence carbon point:
(1) by leek powder 250 DEG C of high temperature carbonization 4h;
(2) product that (1) obtains is mixed with water, obtain dark turbidity liquid;
(3) by dark turbidity liquid whizzer with the centrifugal 10min of 4000r/min rotating speed, then with molecular weight cut-off be 500 ~ 1000Da dialysis tubing dialysis 48h, finally obtain blue-fluorescence carbon point solution.
The fluorescence spectrum figure that embodiment 1 is prepared under the ultraviolet-visible absorption spectroscopy figure of carbon point and different wave length optical excitation is shown in Fig. 1, wherein 1 ~ 6 fluorescence spectrum figure that to be excitation wavelength be respectively under 300nm, 310nm, 320nm, 330nm, 340nm and 350nm excite, 7 is ultraviolet-visible absorption spectroscopy figure.
Embodiment 2
The preparation of blue-fluorescence carbon point:
(1) by leek powder 300 DEG C of high temperature carbonization 3h;
(2) product that (1) obtains is mixed with water, obtain dark turbidity liquid;
(3) by dark turbidity liquid whizzer with the centrifugal 10min of 4000r/min rotating speed, then with molecular weight cut-off be 500 ~ 1000Da dialysis tubing dialysis 48h, finally obtain blue-fluorescence carbon point solution.
The transmission electron microscope picture of the blue-fluorescence carbon point of preparation is shown in Fig. 2.
Embodiment 3
The preparation of blue-fluorescence carbon point:
(1) by leek powder 350 DEG C of high temperature carbonization 2h;
(2) product that (1) obtains is mixed with water, obtain dark turbidity liquid;
(3) by dark turbidity liquid whizzer with the centrifugal 10min of 4000r/min rotating speed, then with molecular weight cut-off be 500 ~ 1000Da dialysis tubing dialysis 48h, finally obtain blue-fluorescence carbon point solution.
The infrared spectrogram of the blue-fluorescence carbon point of preparation is shown in Fig. 3, as can be seen from the figure, and 3420cm
-1and 2928cm
-1peak belongs to O-H and CH
2stretching vibration, 1670cm
-1peak belongs to the stretching vibration of C=O group, 1625cm
-1and 1600cm
-1peak belongs to the stretching vibration of C=C group, 1400cm
-1and 1339cm
-1peak belongs to CH
2the flexural vibration of group, 1260cm
-1and 1121cm
-1peak belongs to the flexural vibration of C-O group, shows that there is a lot of carboxyls on carbon point surface.
Embodiment 4
The preparation of green fluorescence carbon point:
(1) 0.5g leek powder is added in 5mL deionized water, obtained mixed solution;
(2) mixed solution that (1) obtains is transferred in hydrothermal reaction kettle, hydro-thermal reaction 4h at 200 DEG C;
(3) product (2) obtained through centrifugal, dialysis, with whizzer with the centrifugal 10min of 4000r/min rotating speed, then with molecular weight cut-off be 500 ~ 1000Da dialysis tubing dialyse 48h, finally obtain green fluorescence carbon point solution.
The fluorescence spectrum figure prepared under the ultraviolet-visible absorption spectroscopy figure of carbon point and different wave length optical excitation is shown in Fig. 4, wherein 1 ~ 7 fluorescence spectrum figure that to be excitation wavelength be respectively under 400nm, 410nm, 420nm, 430nm, 440nm, 450nm and 460nm excite, 8 is ultraviolet-visible absorption spectroscopy figure.
Embodiment 5
The preparation of green fluorescence carbon point:
(1) 0.5g leek powder is added in 25mL deionized water, obtained mixed solution;
(2) mixed solution that (1) obtains is transferred in hydrothermal reaction kettle, hydro-thermal reaction 3h at 250 DEG C;
(3) product (2) obtained through centrifugal, dialysis, with whizzer with the centrifugal 10min of 4000r/min rotating speed, then with molecular weight cut-off be 500 ~ 1000Da dialysis tubing dialyse 48h, finally obtain green fluorescence carbon point solution.
The transmission electron microscope picture of the blue-fluorescence carbon point of preparation is shown in Fig. 5.
Embodiment 6
The preparation of green fluorescence carbon point:
(1) 0.5g leek powder is added in 50mL deionized water, obtained mixed solution;
(2) mixed solution that (1) obtains is transferred in hydrothermal reaction kettle, hydro-thermal reaction 2h at 300 DEG C;
(3) product (2) obtained through centrifugal, dialysis, with whizzer with the centrifugal 10min of 4000r/min rotating speed, then with molecular weight cut-off be 500 ~ 1000Da dialysis tubing dialyse 48h, finally obtain green fluorescence carbon point solution.
The infrared spectrogram of the green fluorescence carbon point of preparation is shown in Fig. 6, as can be seen from the figure, and 3400cm
-1and 2971cm
-1peak belongs to O-H and CH
2stretching vibration, 1670cm
-1and 1591cm
-1peak belongs to the stretching vibration of C=O and C=C group respectively, 1457cm
-1and 1405cm
-1peak belongs to CH
2the flexural vibration of group, 1300cm
-1and 1124cm
-1peak belongs to the flexural vibration of C-O group, shows that there is a lot of carboxyls on carbon point surface.
Embodiment 7
The application experiment of fluorescent carbon point in cell imaging prepared by embodiment 1 and embodiment 4:
(1) be inoculated in 6 orifice plates by human cervical cancer 1 epidermoid carcinoma cell (A193), every hole adds confining liquid, puts it in wet box, then puts into 37 DEG C, 5%CO
230min is hatched in incubator;
(2) take out 6 orifice plates, first use 0.01molL
-1phosphoric acid buffer wash away confining liquid, then with filter paper, orifice plate surrounding liquid to be blotted;
(3) fluorescent carbon point prepared by embodiment 1 and embodiment 4 is added in 6 orifice plates respectively, at 37 DEG C, 5%CO
230min is hatched altogether in incubator;
(4) 0.01molL is used
-1phosphoric acid buffer washing, be then placed in fluorescence microscopy Microscopic observation carbon point and cell marking situation.
The shows fluorescent microscopy images that embodiment 1 and embodiment 4 prepare carbon point mark human cervical cancer 1 epidermoid carcinoma cell (A193) is shown in Fig. 7, wherein (a) prepares carbon point labeled cell fluorescence imaging (excitation wavelength is 405nm) for embodiment 1, and (b) prepares carbon point labeled cell fluorescence imaging (excitation wavelength is 488nm) for embodiment 4; As can be seen from the figure, cell presents bright blueness and green fluorescence, illustrates that blueness prepared by the present invention and green fluorescence carbon point can as biological fluorescent labeling and optical imagery tag application.
Embodiment 8
The application experiment of fluorescent carbon point in phosphor pattern making prepared by embodiment 2 and embodiment 5:
The fluorescent carbon point aqueous solution prepared by embodiment 2 and embodiment 5 is loaded in pen, filter paper is depicted various pattern, and under then pattern being placed on ultraviolet lamp, in (365nm) and multispectral living body fluorescent molecular image imaging system, (470nm) observes and takes pictures.
Embodiment 2 and embodiment 5 are prepared the figure that carbon point makes for phosphor pattern and are seen Fig. 8, wherein (a) prepares carbon point for design producing (excitation wavelength is 365nm) for embodiment 2, and (b) prepares carbon point for design producing (excitation wavelength is 470nm) for embodiment 5; Blueness bright as we can see from the figure and green fluorescence pattern, illustrate that blueness prepared by the present invention and green fluorescence carbon point have a good application prospect as fluorescent ink.
Embodiment 9
The application experiment of fluorescent carbon point in fluorescent dye prepared by embodiment 3 and embodiment 6:
Be positioned over by various sample in the carbon point aqueous solution obtained by embodiment 3 and embodiment 6 and dye, under then sample being placed on ultraviolet lamp, in (365nm) and multispectral living body fluorescent molecular image imaging system, (470nm) observes and takes pictures.
Embodiment 3 and embodiment 6 are prepared carbon point and are seen Fig. 9 for the figure of fluorescent dye, wherein (a) prepares carbon point for fluorescent dye (excitation wavelength is 365nm) for embodiment 3, and (b) prepares carbon point for fluorescent dye (excitation wavelength is 470nm) for embodiment 6; As we can see from the figure, the sample after carbon Vertex Coloring presents bright blueness and green fluorescence, illustrates that blueness prepared by the present invention and green fluorescence carbon point have potential using value in false proof.
Claims (10)
1. a preparation method for blue-fluorescence carbon point, is characterized in that comprising the steps:
(1) leek powder metallurgy is carbonized;
(2) product that (1) obtains is mixed with water, obtain dark turbidity liquid;
(3) by dark turbidity liquid through centrifugal, dialysis, finally obtain blue-fluorescence carbon point solution.
2. the preparation method of a kind of blue-fluorescence carbon point as claimed in claim 1, is characterized in that, the temperature of step (1) described high temperature carbonization is 250 ~ 350 DEG C, continues 2 ~ 4h.
3. the preparation method of a kind of blue-fluorescence carbon point as claimed in claim 1, is characterized in that, centrifugal described in step (3) is with the centrifugal 10min of 4000r/min rotating speed.
4. the preparation method of a kind of blue-fluorescence carbon point as claimed in claim 1, is characterized in that, the dialysis described in step (3) be with molecular weight cut-off be 500 ~ 1000Da dialysis tubing dialysis 48h.
5. a preparation method for green fluorescence carbon point, is characterized in that comprising the steps:
(1) leek powder is added in deionized water, obtained mixed solution;
(2) mixed solution that (1) obtains is transferred in hydrothermal reaction kettle, carry out hydro-thermal reaction;
(3) product (2) obtained, through centrifugal, dialysis, finally obtains green fluorescence carbon point solution.
6. the preparation method of a kind of green fluorescence carbon point as claimed in claim 5, it is characterized in that, the leek powder described in step (1) mixes 1:10 ~ 100 in mass ratio with deionized water.
7. the preparation method of a kind of green fluorescence carbon point as claimed in claim 5, it is characterized in that, described in step (2), the temperature of hydro-thermal reaction is 200 ~ 300 DEG C, continues 2 ~ 4h.
8. the preparation method of a kind of green fluorescence carbon point as claimed in claim 5, is characterized in that, centrifugal described in step (3) is with the centrifugal 10min of 4000r/min rotating speed.
9. the preparation method of a kind of green fluorescence carbon point as claimed in claim 5, is characterized in that, the dialysis described in step (3) be with molecular weight cut-off be 500 ~ 1000Da dialysis tubing dialysis 48h.
10. the application of the fluorescent carbon point that as described in claim as arbitrary in claim 1-9 prepared by method in cell imaging, phosphor pattern making and fluorescent dye.
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| CN105273715A (en) * | 2015-10-29 | 2016-01-27 | 东华大学 | Method for continuously preparing fluorescent carbon nanoparticles |
| CN105502339A (en) * | 2015-12-28 | 2016-04-20 | 江南大学 | Method for hydro-thermal synthesis of carbon quantum dots with fresh ginger as raw material |
| CN105905884A (en) * | 2016-04-23 | 2016-08-31 | 哈尔滨师范大学 | Preparation method and application of fluorescence carbon quantum dots |
| CN106967425A (en) * | 2016-11-23 | 2017-07-21 | 云南省烟草公司文山州公司 | Using cigarette stalk as the preparation method and application of the fluorescent carbon quantum dot of raw material |
| CN107603608A (en) * | 2017-08-29 | 2018-01-19 | 哈尔滨工业大学 | A kind of method that fluorescent carbon point is prepared using gynostemma pentaphylla as carbon source |
| CN108101023A (en) * | 2017-12-27 | 2018-06-01 | 重庆文理学院 | A kind of method that multi-element doping carbon material is prepared using leek |
| CN109181689A (en) * | 2018-09-26 | 2019-01-11 | 东华大学 | A kind of preparation method of photochromic adjustable hydrophobicity N doping fluorescent carbon point |
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105273715A (en) * | 2015-10-29 | 2016-01-27 | 东华大学 | Method for continuously preparing fluorescent carbon nanoparticles |
| CN105502339A (en) * | 2015-12-28 | 2016-04-20 | 江南大学 | Method for hydro-thermal synthesis of carbon quantum dots with fresh ginger as raw material |
| CN105905884A (en) * | 2016-04-23 | 2016-08-31 | 哈尔滨师范大学 | Preparation method and application of fluorescence carbon quantum dots |
| CN106967425A (en) * | 2016-11-23 | 2017-07-21 | 云南省烟草公司文山州公司 | Using cigarette stalk as the preparation method and application of the fluorescent carbon quantum dot of raw material |
| CN107603608A (en) * | 2017-08-29 | 2018-01-19 | 哈尔滨工业大学 | A kind of method that fluorescent carbon point is prepared using gynostemma pentaphylla as carbon source |
| CN107603608B (en) * | 2017-08-29 | 2020-11-17 | 哈尔滨工业大学 | Method for preparing fluorescent carbon dots by taking gynostemma pentaphylla as carbon source |
| CN108101023A (en) * | 2017-12-27 | 2018-06-01 | 重庆文理学院 | A kind of method that multi-element doping carbon material is prepared using leek |
| CN109181689A (en) * | 2018-09-26 | 2019-01-11 | 东华大学 | A kind of preparation method of photochromic adjustable hydrophobicity N doping fluorescent carbon point |
| CN109181689B (en) * | 2018-09-26 | 2021-09-21 | 东华大学 | Preparation method of photochromic adjustable hydrophobic nitrogen-doped fluorescent carbon dots |
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Application publication date: 20150923 |