CN104031642A - Fluorescence carbon quantum dots, and preparation method and application thereof - Google Patents
Fluorescence carbon quantum dots, and preparation method and application thereof Download PDFInfo
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- CN104031642A CN104031642A CN201410285698.6A CN201410285698A CN104031642A CN 104031642 A CN104031642 A CN 104031642A CN 201410285698 A CN201410285698 A CN 201410285698A CN 104031642 A CN104031642 A CN 104031642A
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Abstract
The invention discloses high-quantum-yield fluorescence carbon quantum dots and a preparation method thereof. The method comprises the following steps: by using chitosan as a carbon source, adding glacial acetic acid and ethylenediamine, and sufficiently stirring to obtain a paste; reacting in a microwave oven to finally obtain a black solid; taking out, naturally cooling, adding a certain amount of secondary water, dissolving by stirring to obtain a brown solution, removing the insoluble substance to obtain a brown solution, dialyzing to remove impurities to obtain a fluorescence carbon quantum dot water solution, and carrying out freeze-drying to obtain the fluorescence carbon quantum dots. The method has the advantages of simple technique, wide raw material sources, low price, low requirements for preparation conditions and higher quantum yield of the obtained carbon quantum dots. The obtained fluorescence carbon quantum dots can be used for detecting Fe<3+> in a water body, and can also be used in living cell fluorescence imaging.
Description
Technical field
The present invention relates to Illuminant nanometer material, relate in particular to carbon quantum dot, specifically fluorescent carbon quantum dot of a kind of high quantum production rate and its preparation method and application.
Background technology
Carbon quantum dot (carbon dots, C-Dots) be by (J Am.Chem.Soc. such as Scrivens, 2004, 126, a kind of novel nano-material taking carbon as skeleton structure of 12736-12737) finding first in the time of research Single Walled Carbon Nanotube in 2004, compare with organic dye with traditional semiconductor-quantum-point, carbon quantum dot as one is novel can luminescent material, not only keep 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 easily extensive incomparable advantage such as synthetic, and damaging cells not substantially, especially in the time of mark living body biological, there is unique advantage, be subject at present extensive concern.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 can realize up-conversion fluorescence transmitting, the most important thing is, carbon quantum dot fluorescent material more in the past has more biological safe type, embodies important value in fields such as biochemical analysis, biosensor, opto-electronic conversion and the photochemical catalysis of fluorescent probe biological detection, bio-sensing, bioanalysis, metallic cation and negatively charged ion.
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, peel off from larger carbon structure the physical method of preparing carbon nano-particle, by the mode of polymer surfaces passivation, it is effectively given out light 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 of acquisition carbon quantum dot is lower; Synthetic method from bottom to top, by pyrolysis or the suitable directly synthetic fluorescent carbon quantum dot of precursor of carbonization, comprise combustion method, hydrothermal solution carborization, support synthesis method, microwave method, supersonic method etc., but the raw material of selecting due to these class methods 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 cheap and easy to get, Nantural non-toxic, it is particularly important that the fluorescent carbon quantum dot that utilizes simple and easy effective means to prepare fast excellent in optical properties seems.In addition, expand the Application Areas of carbon quantum dot 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 the preparation method of the cheap and environmental protection of a kind of simple to operate, device simple, raw material; And described fluorescent carbon quantum dot is used for to 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), chitosan is placed in to 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), the resistance to microwave container that pasty substance is housed is placed in to microwave oven, under high fiery state, react 12-18min, obtain brownish black solid;
3), take out resistance to microwave container, naturally cooling, add the overall accumulated amount 1-2 of Glacial acetic acid and quadrol intermediate water doubly, stirring and dissolving obtains brown solution, filter the brown solution that removal insolubles obtains clarification, by the dialysis tubing of 500-1000Da, dialysis treatment at least 3 days in Glass Containers, obtains the aqueous solution of pure fluorescent carbon quantum dot;
4), will after the lyophilize of the above-mentioned fluorescent carbon quantum dot aqueous solution, obtain target fluorescent carbon quantum dot.
The fluorescent carbon quantum dot that above-mentioned preparation method makes, Fe
3+, there is non-radiative transfer transport in the carbon quantum dot effect with rich surface phenolic hydroxy group, causes the quencher of carbon quantum dot fluorescence, can be used as Fe in water body
3+detection; This fluorescent carbon quantum dot median size little (< 5 nanometers), cytotoxicity are low, and it can permeates cell membranes enter tenuigenin, can in viable cell fluorescence imaging, apply.
Compared with prior art advantage of the present invention:
(1) the present invention is simple to operate, does not need follow-up strong acid or surface passivation agent processing, and a step can obtain high-fluorescence quantum yield carbon quantum dot.
(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 in tens minutes, complete fast energy-and time-economizing.
(4) quantum yield of carbon quantum dot is higher, and taking Quinine Sulphate Di HC (quantum yield 54%) as object of reference, gained carbon quantum dot obtains Relative quantum yields generally between 12.2%～20.0%.
In a word; technological operation of the present invention is simple; raw material sources extensively and low price; preparation condition requires low and relatively gentle; gained carbon quantum dot quantum yield is higher; having solved existing carbon quantum dot preparation method cannot large-scale production and obtain the lower problem of fluorescence quantum yield of carbon quantum dot because of the restriction of technique and raw material, and this carbon quantum dot can be applicable to the fields such as metal ion detection, biomarker, Biological imaging, optoelectronic equipment and biosensor.
Brief description of the drawings
Fig. 1 is ultra-violet absorption spectrum and the fluorescence emission spectrum of the fluorescent carbon quantum dot prepared of 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 fluorescent emission curve prepared of embodiment 1 changes with excitation wavelength
Fig. 3 is taking 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 the fluorescent carbon quantum dot prepared of embodiment 1, and in figure, X-coordinate is for detecting wavelength, and ordinate zou is transmitance;
Fig. 5 is the XRD spectrum figure of the fluorescent carbon quantum dot prepared of embodiment 1;
Fig. 6 is the XPS spectrum figure of the fluorescent carbon quantum dot prepared of embodiment 1.
Fig. 7 is transmission electron microscope picture (left side) and the size distribution figure (right side) of the fluorescent carbon quantum dot prepared of 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 fluorescent carbon quantum dot prepared by embodiment 1 utilizes mtt assay to carry out;
Figure 10 is that 786-0 (kidney clear cell adenocarcinoma) the laser co-focusing figure of the fluorescent carbon quantum dot mark prepared of embodiment 1 is (in figure: (a) be light field gray-scale map; (b) be the details in a play not acted out on stage, but told through dialogues figure of 408nm under exciting, cell presents blue-fluorescence; (c) be (a) and stacking diagram (b); (d) be the details in a play not acted out on stage, but told through dialogues figure of 488nm under exciting, cell presents green fluorescence; (e) be the details in a play not acted out on stage, but told through dialogues figure of 550nm under exciting, cell presents red fluorescence).
Embodiment
Below in conjunction with embodiment, the present invention is elaborated, embodiment has provided 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 subsequently 10mL8% Glacial acetic acid and 5mL ethylenediamine solution, fully stirs, and obtains pasty substance;
Step 2, is placed in resistance to microwave container under the high fiery state of microwave oven (700 watts) and reacts 15min, obtains black solid;
Step 3, takes out resistance to microwave container, and naturally cooling adds 20mL intermediate water wherein, and stirring and dissolving obtains brown solution, filters removal insolubles and obtains the brown solution of clarifying, and removes impurity by dialysis, obtains the aqueous solution of pure fluorescent carbon quantum dot;
Step 4, will obtain fluorescent carbon quantum dot 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 are shown in property representation and application.
Embodiment 2
Step 1, weighs 2g chitosan in resistance to microwave container, adds subsequently 20mL4% Glacial acetic acid and 10mL ethylenediamine solution, fully stirs, and obtains pasty substance;
Step 2, is placed in resistance to microwave container under the high fiery state of microwave oven (700 watts) and reacts 17min, obtains black solid;
Step 3, takes out resistance to microwave container, and naturally cooling adds 40mL intermediate water wherein, and stirring and dissolving obtains brown solution, filters removal insolubles and obtains the brown solution of clarifying, and removes impurity by dialysis, obtains the aqueous solution of pure fluorescent carbon quantum dot;
Step 4, will obtain high-fluorescence quantum yield carbon quantum dot 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 subsequently 8mL8% Glacial acetic acid and 7mL ethylenediamine solution, fully stirs, and obtains pasty substance;
Step 2, is placed in resistance to microwave container under the high fiery state of microwave oven (700 watts) and reacts 12min, obtains black solid;
Step 3, takes out resistance to microwave container, and naturally cooling adds 20mL intermediate water wherein, and stirring and dissolving obtains brown solution, filters removal insolubles and obtains the brown solution of clarifying, and removes impurity by dialysis, obtains the aqueous solution of pure fluorescent carbon quantum dot;
Step 4, will obtain high-fluorescence quantum yield carbon quantum dot 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 subsequently 8mL2% Glacial acetic acid and 7mL ethylenediamine solution, fully stirs, and obtains pasty substance;
Step 2, is placed in resistance to microwave container under the high fiery state of microwave oven (700 watts) and reacts 13min, obtains black solid;
Step 3, takes out resistance to microwave container, and naturally cooling adds 20mL intermediate water wherein, and stirring and dissolving obtains brown solution, filters removal insolubles and obtains the brown solution of clarifying, and removes impurity by dialysis, obtains the aqueous solution of pure fluorescent carbon quantum dot;
Step 4, will obtain high-fluorescence quantum yield carbon quantum dot 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 subsequently 30mL2% Glacial acetic acid and 15mL ethylenediamine solution, fully stirs, and obtains pasty substance;
Step 2, is placed in resistance to microwave container under the high fiery state of microwave oven (700 watts) and reacts 18min, obtains black solid;
Step 3, takes out resistance to microwave container, and naturally cooling adds 60mL intermediate water wherein, and stirring and dissolving obtains brown solution, filters removal insolubles and obtains the brown solution of clarifying, and removes impurity by dialysis, obtains the aqueous solution of pure fluorescent carbon quantum dot;
Step 4, will obtain high-fluorescence quantum yield carbon quantum dot 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 subsequently 10mL10% Glacial acetic acid and 5mL ethylenediamine solution, fully stirs, and obtains pasty substance;
Step 2, is placed in resistance to microwave container under the high fiery state of microwave oven (700 watts) and reacts 16min, obtains black solid;
Step 3, takes out resistance to microwave container, and naturally cooling adds 20mL intermediate water wherein, and stirring and dissolving obtains brown solution, filters removal insolubles and obtains the brown solution of clarifying, and removes impurity by dialysis, obtains the aqueous solution of pure fluorescent carbon quantum dot;
Step 4, will obtain high-fluorescence quantum yield carbon quantum dot 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 to 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 to microwave oven, under high fiery state, reacts 12-18min, obtain brownish black solid;
3) take out resistance to microwave container, naturally cooling, add the overall accumulated amount 1-2 of Glacial acetic acid and quadrol intermediate water doubly, stirring and dissolving obtains brown solution, filter the brown solution that removal insolubles obtains clarification, by the dialysis tubing of 500-1000Da, dialysis treatment at least 3 days in Glass Containers, obtains the aqueous solution of pure fluorescent carbon quantum dot;
4) will after the lyophilize of the above-mentioned fluorescent carbon quantum dot aqueous solution, obtain target fluorescent carbon quantum dot.
2. the fluorescent carbon quantum dot that preparation method makes as claimed in claim 1.
3. fluorescent carbon quantum dot as claimed in claim 2 is for water body Fe
3+detection.
4. the application of fluorescent carbon quantum dot as claimed in claim 2 in viable cell fluorescence imaging.
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