CN104031642B - A kind of fluorescent carbon quantum dot and its preparation method and application - Google Patents
A kind of fluorescent carbon quantum dot and its preparation method and application Download PDFInfo
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- CN104031642B CN104031642B CN201410285698.6A CN201410285698A CN104031642B CN 104031642 B CN104031642 B CN 104031642B CN 201410285698 A CN201410285698 A CN 201410285698A CN 104031642 B CN104031642 B CN 104031642B
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Abstract
The invention provides fluorescent carbon quantum dot of a kind of high quantum production rate and preparation method thereof.Preparation process: be carbon source with chitosan, adds Glacial acetic acid and quadrol, fully stirs, obtain pasty substance; Be placed in microwave oven and react, finally obtain black solid; Taking-up is after its naturally cooling, and add a certain amount of intermediate water, stirring and dissolving obtains brown solution, and remove insolubles and obtain brown solution, impurity is removed in dialysis, namely obtains the fluorescent carbon quantum dot aqueous solution, obtains fluorescent carbon quantum dot after lyophilize.Present invention process is simple, and extensively and low price, preparation condition requires low raw material sources, and gained carbon quantum dot quantum yield is higher.The fluorescent carbon quantum dot of gained can be used for the detection of Fe3+ in water body, also can apply in live cell fluorescent imaging.
Description
Technical field
The present invention relates to Illuminant nanometer material, particularly relate to carbon quantum dot, specifically a kind of fluorescent carbon quantum dot and its preparation method and application of high quantum production rate.
Background technology
Carbon quantum dot (carbondots, C-Dots) be by (JAm.Chem.Soc. such as Scrivens, 2004, 126, 12736-12737) when research Single Walled Carbon Nanotube in 2004, Late Cambrian a kind of took carbon as the novel nano-material of skeleton structure, compare with organic dye with traditional semiconductor-quantum-point, carbon quantum dot as one is novel can luminescent material, not only maintain carbon material toxicity little, the advantages such as good biocompatibility, and it is adjustable to have light emitting region, two photon absorption cross section is large, fluorescence quantum efficiency is high, good light stability, without optical flare, be easy to functionalization, inexpensive, the advantage that easily extensive synthesis etc. are incomparable, and not damaging cells substantially, especially when marking living body biological, there is unique advantage, be subject to extensive concern at present.The size of this novel fluorescent carbon nano-particles is similar to semiconductor point, median size is less than 10nm, there is very long fluorescence lifetime, and up-conversion fluorescence can be realized launch, the most important thing is, carbon quantum dot fluorescent material more in the past has more biological safe type, embodies important value in the biochemical analysis of fluorescent probe biological detection, bio-sensing, bioanalysis, metallic cation and negatively charged ion, biosensor, the field such as opto-electronic conversion and photochemical catalysis.
The preparation method of carbon quantum dot mainly contains two kinds at present, method and from bottom to top method from top to bottom.Top-down synthetic method, namely the physical method preparing carbon nano-particle is peeled off from larger carbon structure, it is made effectively to give out light by the mode of polymer surfaces passivation again, mainly comprise arc-over, laser ablation, electrochemical oxidation, electron beam irradiation etc., these class methods often need strict experiment condition or the special energy, cost is high, and the fluorescence quantum yield obtaining carbon quantum dot is lower; Synthetic method from bottom to top, namely directly fluorescent carbon quantum dot is synthesized by pyrolysis or the suitable precursor of carbonization, comprise combustion method, hydrothermal solution carborization, support synthesis method, microwave method, supersonic method etc., but the raw material due to such method selection is all Nonrenewable energy resources and needs strict aftertreatment technology, so be also unfavorable for continuing and scale production carbon quantum dot.Therefore, find raw material that is cheap and easy to get, Nantural non-toxic, the fluorescent carbon quantum dot utilizing simple and easy effective means to prepare excellent in optical properties fast seems particularly important.In addition, the Application Areas of carbon quantum dot is expanded and alternative semiconductors quantum dot and organic dye are also problem demanding prompt solutions gradually.
Summary of the invention
The object of the present invention is to provide a kind of fluorescent carbon quantum dot of high quantum production rate, and set up a kind of simple to operate, device simple, raw material are cheap and the preparation method of environmental protection; And described fluorescent carbon quantum dot is used for detection of heavy metal ion and cell imaging.
The preparation method of the fluorescent carbon quantum dot of a kind of high quantum production rate provided by the invention, comprises the steps:
1), by chitosan be placed in resistance to microwave container, add Glacial acetic acid and quadrol, fully stir, obtain pasty substance; The mass ratio of chitosan, Glacial acetic acid and quadrol is: 0.5-5 ︰ 4.0-55 ︰ 3.2-45;
2), by the resistance to microwave container that pasty substance is housed be placed in microwave oven, react 12-18min under high fiery state, obtain brownish black solid;
3), resistance to microwave container is taken out, naturally cooling, add Glacial acetic acid and the overall accumulated amount 1-2 of quadrol intermediate water doubly, stirring and dissolving obtains brown solution, filter the brown solution removed insolubles and obtain clarifying, by the dialysis tubing of 500-1000Da, dialysis treatment at least 3 days in Glass Containers, namely obtains the aqueous solution of pure fluorescent carbon quantum dot;
4), target fluorescent carbon quantum dot is obtained by after the lyophilize of the above-mentioned fluorescent carbon quantum dot aqueous solution.
The fluorescent carbon quantum dot that above-mentioned preparation method obtains, Fe
3+with the carbon quantum dot effect of rich surface phenolic hydroxy group, there is non-radiative electron transfer, cause carbon quantum dot quenching of fluorescence, can be used as Fe in water body
3+detection; This fluorescent carbon quantum dot median size little (< 5 nanometer), cytotoxicity are low, and it permeates cell membranes can enter tenuigenin, can apply in live cell fluorescent imaging.
Compared with prior art advantage of the present invention:
(1) the present invention is simple to operate, and do not need follow-up strong acid or surface passivator process, a step can obtain carbon quantum dot with high fluorescence quantum yield.
(2) starting material chitosan, Glacial acetic acid and quadrol are general reagent, wide material sources, low price.
(3) production unit only needs microwave oven, easy to operate, can complete fast, energy-and time-economizing in tens minutes.
(4) quantum yield of carbon quantum dot is higher, and with Quinine Sulphate Di HC (quantum yield 54%) for object of reference, gained carbon quantum dot obtains Relative quantum yields generally between 12.2% ~ 20.0%.
In a word; present invention process is simple to operate; raw material sources extensively and low price; preparation condition requirement is low and relatively gentle; gained carbon quantum dot quantum yield is higher; solving existing carbon quantum dot preparation method cannot large-scale production and obtain the lower problem of the fluorescence quantum yield of carbon quantum dot because technique and raw material restriction, and this carbon quantum dot can be applicable to the fields such as metal ion detection, biomarker, Biological imaging, optoelectronic equipment and biosensor.
Accompanying drawing explanation
Fig. 1 is ultra-violet absorption spectrum and the fluorescence emission spectrum of fluorescent carbon quantum dot prepared by embodiment 1; Wherein Glass Containers fills the fluorescent carbon quantum dot aqueous solution, is positioned on ultraviolet transmission platform, after 365nm excitation light source excites, sends blue-fluorescence.
Fig. 2 is the spectrogram that the fluorescent carbon quantum dot fluorescence emission curves of embodiment 1 preparation changes with excitation wavelength
Fig. 3 take Quinine Sulphate Di HC as standard, the quantum yield (left side is Quinine Sulphate Di HC, and right side is carbon quantum dot) of linear fit Quinine Sulphate Di HC and carbon quantum dot;
Fig. 4 is the infrared spectrogram of fluorescent carbon quantum dot prepared by embodiment 1, and in figure, X-coordinate is determined wavelength, and ordinate zou is transmitance;
Fig. 5 is the XRD spectrum figure of fluorescent carbon quantum dot prepared by embodiment 1;
Fig. 6 is the XPS spectrum figure of fluorescent carbon quantum dot prepared by embodiment 1.
Fig. 7 is transmission electron microscope picture (left side) and the grain size distribution (right side) of fluorescent carbon quantum dot prepared by embodiment 1;
Fig. 8 is Fe
3+the fluorescence spectrum figure of fluorescent carbon quantum dot prepared by quencher embodiment 1;
Fig. 9 is 786-0 (kidney clear cell adenocarcinoma) toxotest that the fluorescent carbon quantum dot of embodiment 1 preparation utilizes mtt assay to carry out;
Figure 10 is that 786-0 (kidney clear cell adenocarcinoma) the laser co-focusing figure of fluorescent carbon quantum dot mark prepared by embodiment 1 is (in figure: (a) is light field gray-scale map; (b) for 408nm excite under details in a play not acted out on stage, but told through dialogues figure, cell presents blue-fluorescence; C () is the stacking diagram of (a) and (b); (d) for 488nm excite under details in a play not acted out on stage, but told through dialogues figure, cell presents green fluorescence; (e) for 550nm excite under details in a play not acted out on stage, but told through dialogues figure, cell presents red fluorescence).
Embodiment
Elaborate to the present invention below in conjunction with embodiment, embodiment gives detailed embodiment and concrete operating process, but protection scope of the present invention is not limited to following embodiment.
Embodiment 1
Step 1, weighs 1g chitosan in resistance to microwave container, adds 10mL8% Glacial acetic acid and 5mL ethylenediamine solution subsequently, fully stir, obtain pasty substance;
Step 2, reacts 15min under resistance to microwave container being placed in microwave oven (700 watts) high fiery state, obtains black solid;
Step 3, takes out resistance to microwave container, naturally cooling, and add 20mL intermediate water wherein, stirring and dissolving obtains brown solution, filters the brown solution removed insolubles and obtain clarifying, removes impurity, namely obtain the aqueous solution of pure fluorescent carbon quantum dot by dialysis;
Step 4, obtains fluorescent carbon quantum dot by after the lyophilize of the above-mentioned fluorescent carbon quantum dot aqueous solution, and its Relative quantum yields (taking Quinine Sulphate Di HC as standard) is 19.5%.
Fig. 1-10 is shown in property representation and application.
Embodiment 2
Step 1, weighs 2g chitosan in resistance to microwave container, adds 20mL4% Glacial acetic acid and 10mL ethylenediamine solution subsequently, fully stir, obtain pasty substance;
Step 2, reacts 17min under resistance to microwave container being placed in microwave oven (700 watts) high fiery state, obtains black solid;
Step 3, takes out resistance to microwave container, naturally cooling, and add 40mL intermediate water wherein, stirring and dissolving obtains brown solution, filters the brown solution removed insolubles and obtain clarifying, removes impurity, namely obtain the aqueous solution of pure fluorescent carbon quantum dot by dialysis;
Step 4, obtains carbon quantum dot with high fluorescence quantum yield by after the lyophilize of the above-mentioned fluorescent carbon quantum dot aqueous solution, and its Relative quantum yields (taking Quinine Sulphate Di HC as standard) is 16.6%.
Embodiment 3
Step 1, weighs 1g chitosan in resistance to microwave container, adds 8mL8% Glacial acetic acid and 7mL ethylenediamine solution subsequently, fully stir, obtain pasty substance;
Step 2, reacts 12min under resistance to microwave container being placed in microwave oven (700 watts) high fiery state, obtains black solid;
Step 3, takes out resistance to microwave container, naturally cooling, and add 20mL intermediate water wherein, stirring and dissolving obtains brown solution, filters the brown solution removed insolubles and obtain clarifying, removes impurity, namely obtain the aqueous solution of pure fluorescent carbon quantum dot by dialysis;
Step 4, obtains carbon quantum dot with high fluorescence quantum yield by after the lyophilize of the above-mentioned fluorescent carbon quantum dot aqueous solution, and its Relative quantum yields (taking Quinine Sulphate Di HC as standard) is 17.1%.
Embodiment 4
Step 1, weighs 1g chitosan in resistance to microwave container, adds 8mL2% Glacial acetic acid and 7mL ethylenediamine solution subsequently, fully stir, obtain pasty substance;
Step 2, reacts 13min under resistance to microwave container being placed in microwave oven (700 watts) high fiery state, obtains black solid;
Step 3, takes out resistance to microwave container, naturally cooling, and add 20mL intermediate water wherein, stirring and dissolving obtains brown solution, filters the brown solution removed insolubles and obtain clarifying, removes impurity, namely obtain the aqueous solution of pure fluorescent carbon quantum dot by dialysis;
Step 4, obtains carbon quantum dot with high fluorescence quantum yield by after the lyophilize of the above-mentioned fluorescent carbon quantum dot aqueous solution, and its Relative quantum yields (taking Quinine Sulphate Di HC as standard) is 12.5%.
Embodiment 5
Step 1, weighs 3g chitosan in beaker, adds 30mL2% Glacial acetic acid and 15mL ethylenediamine solution subsequently, fully stir, obtain pasty substance;
Step 2, reacts 18min under resistance to microwave container being placed in microwave oven (700 watts) high fiery state, obtains black solid;
Step 3, takes out resistance to microwave container, naturally cooling, and add 60mL intermediate water wherein, stirring and dissolving obtains brown solution, filters the brown solution removed insolubles and obtain clarifying, removes impurity, namely obtain the aqueous solution of pure fluorescent carbon quantum dot by dialysis;
Step 4, obtains carbon quantum dot with high fluorescence quantum yield by after the lyophilize of the above-mentioned fluorescent carbon quantum dot aqueous solution, and its Relative quantum yields (taking Quinine Sulphate Di HC as standard) is 18.0%.
Embodiment 6
Step 1, weighs 1g chitosan in resistance to microwave container, adds 10mL10% Glacial acetic acid and 5mL ethylenediamine solution subsequently, fully stir, obtain pasty substance;
Step 2, reacts 16min under resistance to microwave container being placed in microwave oven (700 watts) high fiery state, obtains black solid;
Step 3, takes out resistance to microwave container, naturally cooling, and add 20mL intermediate water wherein, stirring and dissolving obtains brown solution, filters the brown solution removed insolubles and obtain clarifying, removes impurity, namely obtain the aqueous solution of pure fluorescent carbon quantum dot by dialysis;
Step 4, obtains carbon quantum dot with high fluorescence quantum yield by after the lyophilize of the above-mentioned fluorescent carbon quantum dot aqueous solution, and its Relative quantum yields (taking Quinine Sulphate Di HC as standard) is 18.7%.
Claims (4)
1. a preparation method for the fluorescent carbon quantum dot of high quantum production rate, is characterized in that, comprises the following steps:
1) chitosan is placed in resistance to microwave container, adds Glacial acetic acid and quadrol, fully stir, obtain pasty substance; The mass ratio of chitosan, Glacial acetic acid and quadrol is 0.5-5 ︰ 4.0-55 ︰ 3.2-45;
2) the resistance to microwave container that pasty substance is housed is placed in microwave oven, reacts 12-18min under high fiery state, obtain brownish black solid;
3) resistance to microwave container is taken out, naturally cooling, add Glacial acetic acid and the overall accumulated amount 1-2 of quadrol intermediate water doubly, stirring and dissolving obtains brown solution, filter the brown solution removed insolubles and obtain clarifying, by the dialysis tubing of 500-1000Da, dialysis treatment at least 3 days in Glass Containers, namely obtains the aqueous solution of pure fluorescent carbon quantum dot;
4) target fluorescent carbon quantum dot is obtained by after the lyophilize of the above-mentioned fluorescent carbon quantum dot aqueous solution.
2. the fluorescent carbon quantum dot that obtains of preparation method as claimed in claim 1.
3. fluorescent carbon quantum dot as claimed in claim 2 is used for Fe in water body
3+detection.
4. the application of fluorescent carbon quantum dot in live cell fluorescent imaging as claimed in claim 2.
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