CN103387219A - A preparation method for water-soluble multicolor carbon quantum points by microwave radiation - Google Patents
A preparation method for water-soluble multicolor carbon quantum points by microwave radiation Download PDFInfo
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- CN103387219A CN103387219A CN2013103082507A CN201310308250A CN103387219A CN 103387219 A CN103387219 A CN 103387219A CN 2013103082507 A CN2013103082507 A CN 2013103082507A CN 201310308250 A CN201310308250 A CN 201310308250A CN 103387219 A CN103387219 A CN 103387219A
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Abstract
The invention discloses a preparation method for water-soluble multicolor carbon quantum points by microwave radiation. A precursor solution is prepared by uniformly mixing an organic carbon source and ultrapure water, and is put into a glass tube specialized for microwave radiation, and microwave radiation is performed in a microwave reactor to prepare the water-soluble multicolor carbon quantum points. The method is performed completely in a water phase, and the method has safe operation, speediness, convenience, small toxicity and easily available and safe raw materials. The water-soluble multicolor carbon quantum points have good monodispersity, good fluorescence property, high quantum yield, good stability and good water solubility. The water-soluble multicolor carbon quantum points can be used for biological detection and analyses as fluorescence indicators.
Description
Technical field
The invention belongs to nano material and bioanalysis detection technique field, be specifically related to a kind of microwave radiation preparation of water-soluble polychrome carbon quantum dot.
Background technology
The carbon quantum dot with its unreactiveness, optical flare lack, the photobleaching rate is low, toxicity is low, good biocompatibility obtains increasing the concern.Than organic dye and the quantum dot that contains heavy metal ion, the carbon quantum dot can be applied to a plurality of fields, such as bio-imaging, photochemical catalysis, detection, laser, LED, energy storage and transition device etc.In the recent period the progress in carbon quantum dot synthetic method field makes the carbon quantum dot to make by method (top-down) from top to bottom via perfect carbon structure (such as graphene, multi-walled carbon nano-tubes), or via the chemical substance (such as ammonium citrate and ethylenediamine tetraacetic acid (EDTA)) of carbon containing, by method (down-top) from top to bottom, makes.It should be noted that carbon quantum dot that these methods make all needs surface oxidation or the passivation can be luminous and possess water-soluble.In addition, the single stage method carbon quantum dot for preparing surface passivation also has report.In these methods, microwave process for synthesizing is especially outstanding because it have start quick, heating is easy to control, even etc. the advantage of heat-processed.Recently, the near-infrared luminous CdTe quantum dot (Angew.Chem.Int.Ed.2011 that is prepared by microwave method, 50,5695-5698), multicolor luminous silicon nanowires (Angew.Chem.2011,123,3136-3139), biological functionality fluorescence radiation nano silicon particles (Angew.Chem.Int.Ed.2012,51,8485 – 8489) and water-soluble super light is stable and PH stability silicon quantum dot (J.Am.Chem.Soc.2011,133,14192-14195) by the contriver, successfully synthesized.
Summary of the invention
The object of the present invention is to provide a kind of operational safety, single stage method microwave radiation fast and convenient, with low cost to prepare the method for water-soluble polychrome carbon quantum dot, the polychrome carbon quantum dot of gained can be used to cell and the living imaging of high spatial resolution.
For achieving the above object, the invention provides following technical scheme:
Microwave radiation of the present invention prepares the method for water-soluble polychrome carbon quantum dot, specifically comprises the steps:
(1) organic carbon source and ultrapure water evenly are hybridly prepared into precursor solution standby;
(2) with the precursor solution of gained at microwave power 15W～1000W, 150 ℃～180 ℃ lower radiation heating 15min～300min of temperature, obtain water-soluble polychrome carbon quantum dot.
Described organic carbon source can be cheap, be available anywhere, the organic carbonaceous material of green non-pollution, milk, honey, egg, lemon juice, Yulan Magnolia etc.
Preferably, described organic carbon source is milk, and its mixed volume ratio with ultrapure water is 1:10～1:50.
Further, described milk is 1:30 with the mixed volume ratio of ultrapure water.
Microwave radiation of the present invention prepares the method for water-soluble polychrome carbon quantum dot, at aqueous phase, carries out fully, and operational safety, fast and convenient, toxicity is little, and materials safety is easy to get.The water-soluble polychrome carbon quantum dot of gained has good monodispersity, and photoluminescent property and quantum yield are high, and good stability has good water-solublely, can be used as fluorescent marker and is widely used in biological detection and analysis.
Description of drawings
In order to be illustrated more clearly in the technical scheme in the embodiment of the present invention, in below describing embodiment, the accompanying drawing of required use is briefly described, apparently, accompanying drawing relevant of the present invention in the following describes is only some embodiments of the present invention, for those of ordinary skills, under the prerequisite of not paying creative work, can also obtain according to these accompanying drawings other accompanying drawing.
Fig. 1 is ultraviolet-fluorescence (UV-PL) spectrogram of the water-soluble polychrome carbon quantum dot for preparing of the present invention, and wherein, excitation wavelength is 365nm;
Fig. 2 is the fluorescence spectrum figure of the water-soluble polychrome carbon quantum dot for preparing of the present invention, and wherein, excitation wavelength is from 300nm to 500nm, every 20nm, excites once;
Fig. 3 is transmission electron microscope (TEM) figure and high resolving power transmission electron microscope (HRTEM) figure of the water-soluble polychrome carbon quantum dot for preparing of the present invention, and wherein a is TEM figure, and interior figure is that HRTEM schemes; B is the size distribution plot under TEM;
Fig. 4 is that the water-soluble polychrome carbon quantum dot that the present invention prepares is used the Raman spectrogram of the silicon chip of growth in situ silver nano-grain as substrate under drying regime;
Fig. 5 is the infrared spectrum of water-soluble polychrome carbon quantum dot under drying regime that the present invention prepares;
Fig. 6 is the X-ray diffraction spectrogram of water-soluble polychrome carbon quantum dot under drying regime that the present invention prepares.
Embodiment
Below in conjunction with the accompanying drawing in the embodiment of the present invention, the technical scheme in the embodiment of the present invention is described in detail.
The present invention's raw material used can freely be buied by market; Microwave reactor model for the preparation of water-soluble polychrome carbon quantum dot: 8.8, be purchased from the Preekem company in Shanghai.
Embodiment 1
(1) precursor preparation
33 ml milks are poured in the volumetric flask of 1 liter, add ultrapure water to 1 and rise scale marks, obtain carbon quantum dot precursor solution standby;
(2) microwave radiation prepares water-soluble polychrome carbon quantum dot
The carbon quantum dot precursor solution of gained is carried out microwave radiation, can obtain water-soluble polychrome carbon quantum dot.
Condition is: microwave power 600W; Temperature: 170 ℃; Time: 15min.
(1) precursor preparation
33 ml milks are poured in the volumetric flask of 1 liter, add ultrapure water to 1 and rise scale marks, obtain carbon quantum dot precursor solution standby;
(2) microwave radiation prepares water-soluble polychrome carbon quantum dot
The carbon quantum dot precursor solution of gained is carried out microwave radiation, can obtain water-soluble polychrome carbon quantum dot.
Condition is: microwave power 600W; Temperature: 160 ℃; Time: 15min.
Embodiment 3
(1) precursor preparation
33 ml milks are poured in the volumetric flask of 1 liter, add ultrapure water to 1 and rise scale marks, obtain carbon quantum dot precursor solution standby;
(2) microwave radiation prepares water-soluble polychrome carbon quantum dot
The carbon quantum dot precursor solution of gained is carried out microwave radiation, can obtain water-soluble polychrome carbon quantum dot.
Condition is: microwave power 600W; Temperature: 150 ℃; Time: 15min.
Embodiment 4
(1) precursor preparation
33 ml milks are poured in the volumetric flask of 1 liter, add ultrapure water to 1 and rise scale marks, obtain carbon quantum dot precursor solution standby;
(2) microwave radiation prepares water-soluble polychrome carbon quantum dot
The carbon quantum dot precursor solution of gained is carried out microwave radiation, can obtain water-soluble polychrome carbon quantum dot.
Condition is: microwave power 600W; Temperature: 170 ℃; Time: 30min.
Embodiment 5
(1) precursor preparation
33 ml milks are poured in the volumetric flask of 1 liter, add ultrapure water to 1 and rise scale marks, obtain carbon quantum dot precursor solution standby;
(2) microwave radiation prepares water-soluble polychrome carbon quantum dot
The carbon quantum dot precursor solution of gained is carried out microwave radiation, can obtain water-soluble polychrome carbon quantum dot.
Condition is: microwave power 600W; Temperature: 160 ℃; Time: 30min.
Embodiment 6
(1) precursor preparation
33 ml milks are poured in the volumetric flask of 1 liter, add ultrapure water to 1 and rise scale marks, obtain carbon quantum dot precursor solution standby;
(2) microwave radiation prepares polychrome water-soluble carbon quantum dot
The carbon quantum dot precursor solution of gained is carried out microwave radiation, can obtain water-soluble polychrome carbon quantum dot.
Condition is: microwave power 600W; Temperature: 150 ℃; Time: 30min.
Above-mentioned all embodiment are illustrated take organic carbon source as milk, described organic carbon source be cheap, be available anywhere, the organic carbonaceous material of green non-pollution, other are applicable too such as honey, egg, lemon juice, Yulan Magnolia etc.According to the difference of organic carbon source, select to add the ultrapure water of different amounts, regulate suitable viscosity ratio, operate with the instant microwave radiation heating.When using milk during as organic carbon source, its mixed volume with ultrapure water is advisable than with 1:10～1:50, especially take 1:30 as best.
In sum, microwave radiation of the present invention prepares the method for water-soluble polychrome carbon quantum dot, at aqueous phase, carry out fully, and operational safety, fast and convenient, toxicity is little, and materials safety is easy to get.Can be found out by accompanying drawing 1～accompanying drawing 6, the water-soluble polychrome carbon quantum dot of gained has good monodispersity, and photoluminescent property and quantum yield are high, and good stability has good water-solublely, can be used as fluorescent marker and is widely used in biological detection and analysis.
To those skilled in the art, obviously the invention is not restricted to the details of above-mentioned one exemplary embodiment, and in the situation that do not deviate from spirit of the present invention or essential characteristic, can realize the present invention with other specific form.Therefore, no matter from which point, all should regard embodiment as exemplary, and be nonrestrictive, scope of the present invention is limited by claims rather than above-mentioned explanation, therefore is intended to include in the present invention dropping on the implication that is equal to important document of claim and all changes in scope.
In addition, be to be understood that, although this specification sheets is described according to embodiment, but not each embodiment only comprises an independently technical scheme, this narrating mode of specification sheets is only for clarity sake, those skilled in the art should make specification sheets as a whole, and the technical scheme in each embodiment also can, through appropriate combination, form other embodiments that it will be appreciated by those skilled in the art that.
Claims (4)
1. a microwave radiation prepares the method for water-soluble polychrome carbon quantum dot, it is characterized in that, comprises the steps:
(1) organic carbon source and ultrapure water evenly are hybridly prepared into precursor solution standby;
(2) with the precursor solution of gained at microwave power 15W～1000W, 150 ℃～180 ℃ lower radiation heating 15min～300min of temperature, obtain water-soluble polychrome carbon quantum dot.
2. method according to claim 1, it is characterized in that: described organic carbon source is milk, honey, egg, lemon juice or Yulan Magnolia.
3. method according to claim 2, it is characterized in that: described organic carbon source is milk, its with mixed volume of ultrapure water than being 1:10～1:50.
4. method according to claim 3 is characterized in that: the mixed volume of described milk and ultrapure water is than being 1:30.
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