CN103387219B - The method of water-soluble multicolor carbon quantum point prepared by a kind of microwave radiation - Google Patents
The method of water-soluble multicolor carbon quantum point prepared by a kind of microwave radiation Download PDFInfo
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- CN103387219B CN103387219B CN201310308250.7A CN201310308250A CN103387219B CN 103387219 B CN103387219 B CN 103387219B CN 201310308250 A CN201310308250 A CN 201310308250A CN 103387219 B CN103387219 B CN 103387219B
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Abstract
The invention discloses a kind of method that water-soluble multicolor carbon quantum point prepared by microwave radiation, organic carbon source and ultra-pure water are uniformly hybridly prepared into precursor solution be placed in the glass tubing that microwave radiation is special, in microwave reactor, carry out microwave radiation, prepare water-soluble multicolor carbon quantum point.The method of the present invention is carried out completely in aqueous phase, operates safety, and fast and convenient, toxicity is little, and materials safety is easy to get;The water-soluble multicolor carbon quantum point of gained has good monodispersity, photoluminescent property and quantum yield high, and good stability has good water solublity, can be widely used in biological detection and analysis as fluorescent marker.
Description
Technical field
The invention belongs to nano material and bioanalysis detection technique field, be specifically related to a kind of water-soluble multicolor
The microwave radiation preparation of carbon quantum dot.
Background technology
Carbon quantum dot with its chemical inertness, optical flare lack, photobleaching rate is low, toxicity is low, biocompatibility
Good acquisition is more and more paid close attention to.Compared to organic dyestuff and the quantum dot containing heavy metal ion, carbon quantum
Point can apply to multiple field, such as bio-imaging, photocatalysis, detection, laser, LED, energy storage
Deposit and transition device etc..In the recent period the progress in carbon quantum dot synthetic method field makes the carbon quantum dot can be via
Perfect carbon structure (such as graphene, multi-walled carbon nano-tubes) is made by method (top-down) from top to bottom
, or via carbon containing chemical substance (such as ammonium citrate and ethylenediaminetetraacetic acid) by from lower to
Upper method (down-top) prepares.It should be noted that the carbon quantum dot that these methods prepare is required for Surface Oxygen
Change or passivation can be luminous and possess water solublity.It addition, one-step method prepares the carbon quantum of surface passivation
Point also has been reported that.In these methods, microwave process for synthesizing is the most prominent, because it has startup agility, adds
Easy to control, the heating process of heat uniformly etc. advantage.Recently, microwave method the near-infrared luminous CdTe prepared
Quantum dot (Angew.Chem.Int.Ed.2011,50,5695-5698), multicolor luminous silicon nanowires (Angew.
Chem.2011,123,3136-3139), Biofunctional fluorescence radiation nano silicon particles (Angew.Chem.
Int.Ed.2012,51,8485 8489) and the super light of water solublity is stable and PH stability silicon quantum dot (J.
Am.Chem.Soc.2011,133,14192-14195) successfully synthesized by inventor.
Summary of the invention
It is an object of the invention to provide and a kind of operate one-step method microwave safe, fast and convenient, with low cost
The method of radiation preparation water-soluble multicolor carbon quantum point, the multicolor carbon quantum points of gained can be used for high spatial
The cell of resolution and living imaging.
For achieving the above object, the present invention provides following technical scheme:
The method of water-soluble multicolor carbon quantum point prepared by the microwave radiation of the present invention, specifically includes following step:
(1) organic carbon source and ultra-pure water are uniformly hybridly prepared into precursor solution standby;
(2) by the precursor solution of gained spoke at microwave power 15W~1000W, temperature 150 DEG C~180 DEG C
Penetrate heating 15min~300min, obtain water-soluble multicolor carbon quantum point.
Described organic carbon source can be cheap, be available anywhere, the organic carbon containing substances of green non-pollution, cattle
Milk, Mel, egg, Fructus Citri Limoniae juice, Magnolia denudata Desr. etc..
Preferably, described organic carbon source is milk, and its mixed volume with ultra-pure water is than for 1:10~1:50.
Further, the mixed volume of described milk and ultra-pure water is than for 1:30.
The method of water-soluble multicolor carbon quantum point prepared by the microwave radiation of the present invention, carries out in aqueous phase completely,
Operation safety, fast and convenient, toxicity is little, and materials safety is easy to get.The water-soluble multicolor carbon quantum point of gained has
Well monodispersity, photoluminescent property and quantum yield are high, and good stability has good water solublity, can
To be widely used in biological detection and analysis as fluorescent marker.
Accompanying drawing explanation
For the technical scheme being illustrated more clearly that in the embodiment of the present invention, institute in embodiment being described below
The accompanying drawing used is needed to be briefly described, it should be apparent that, the accompanying drawing for the present invention in describing below
It is only some embodiments of the present invention, for those of ordinary skill in the art, is not paying creativeness
On the premise of work, it is also possible to obtain other accompanying drawing according to these accompanying drawings.
Fig. 1 is UV-fluorescence (UV-PL) spectrum of the water-soluble multicolor carbon quantum point that the present invention prepares
Figure, wherein, excitation wavelength is 365nm;
Fig. 2 is the fluorescence spectrum figure of the water-soluble multicolor carbon quantum point that the present invention prepares, and wherein, excites
Wavelength is from 300nm to 500nm, excites once every 20nm;
Fig. 3 is transmission electron microscope (TEM) figure and the height of the water-soluble multicolor carbon quantum point that the present invention prepares
Resolution Transmission Electronic Speculum (HRTEM) figure, wherein a is TEM figure, and interior figure is HRTEM figure;B is
Size distribution plot under TEM;
Fig. 4 is that the water-soluble multicolor carbon quantum point that the present invention prepares is silver-colored with growth in situ in the dry state
The silicon chip of nano-particle is as the Raman spectrogram of substrate;
Fig. 5 is the water-soluble multicolor carbon quantum point for preparing of present invention infrared spectrum in the dry state;
Fig. 6 is the water-soluble multicolor carbon quantum point for preparing of present invention X-ray diffraction in the dry state
Spectrogram.
Detailed description of the invention
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 carried out in detail
Thin description.
Raw material used by the present invention freely can be buied by market;For preparing the micro-of water-soluble multicolor carbon quantum point
Ripple reactor model: 8.8, is purchased from the Preekem company in Shanghai.
Embodiment 1
(1) prepared by precursor
33 milliliters of milk are poured in the volumetric flask of 1 liter, add ultra-pure water to 1 liter of graduation mark, obtain carbon
Quantum dot precursor solution is standby;
(2) water-soluble multicolor carbon quantum point prepared by microwave radiation
The carbon quantum dot precursor solution of gained is carried out microwave radiation, available water-soluble multicolor carbon quantum point.
Condition is: microwave power 600W;Temperature: 170 DEG C;Time: 15min.
Embodiment 2
(1) prepared by precursor
33 milliliters of milk are poured in the volumetric flask of 1 liter, add ultra-pure water to 1 liter of graduation mark, obtain carbon
Quantum dot precursor solution is standby;
(2) water-soluble multicolor carbon quantum point prepared by microwave radiation
The carbon quantum dot precursor solution of gained is carried out microwave radiation, available water-soluble multicolor carbon quantum point.
Condition is: microwave power 600W;Temperature: 160 DEG C;Time: 15min.
Embodiment 3
(1) prepared by precursor
33 milliliters of milk are poured in the volumetric flask of 1 liter, add ultra-pure water to 1 liter of graduation mark, obtain carbon
Quantum dot precursor solution is standby;
(2) water-soluble multicolor carbon quantum point prepared by microwave radiation
The carbon quantum dot precursor solution of gained is carried out microwave radiation, available water-soluble multicolor carbon quantum point.
Condition is: microwave power 600W;Temperature: 150 DEG C;Time: 15min.
Embodiment 4
(1) prepared by precursor
33 milliliters of milk are poured in the volumetric flask of 1 liter, add ultra-pure water to 1 liter of graduation mark, obtain carbon
Quantum dot precursor solution is standby;
(2) water-soluble multicolor carbon quantum point prepared by microwave radiation
The carbon quantum dot precursor solution of gained is carried out microwave radiation, available water-soluble multicolor carbon quantum point.
Condition is: microwave power 600W;Temperature: 170 DEG C;Time: 30min.
Embodiment 5
(1) prepared by precursor
33 milliliters of milk are poured in the volumetric flask of 1 liter, add ultra-pure water to 1 liter of graduation mark, obtain carbon
Quantum dot precursor solution is standby;
(2) water-soluble multicolor carbon quantum point prepared by microwave radiation
The carbon quantum dot precursor solution of gained is carried out microwave radiation, available water-soluble multicolor carbon quantum point.
Condition is: microwave power 600W;Temperature: 160 DEG C;Time: 30min.
Embodiment 6
(1) prepared by precursor
33 milliliters of milk are poured in the volumetric flask of 1 liter, add ultra-pure water to 1 liter of graduation mark, obtain carbon
Quantum dot precursor solution is standby;
(2) polychrome Water-soluble carbon quantum dot prepared by microwave radiation
The carbon quantum dot precursor solution of gained is carried out microwave radiation, available water-soluble multicolor carbon quantum point.
Condition is: microwave power 600W;Temperature: 150 DEG C;Time: 30min.
Above-mentioned all embodiments are illustrated with organic carbon source for milk, described organic carbon source be cheap, with
Place can obtain, the organic carbon containing substances of green non-pollution, other such as Mel, egg, Fructus Citri Limoniae juice, Magnolia denudata Desr.
Etc. be equally applicable.According to the difference of organic carbon source, selecting to add different amounts of ultra-pure water, regulation is suitable
Viscosity ratio, with instant microwave radiate heating operation.When using milk as organic carbon source, it is with ultrapure
The mixed volume of water is advisable than with 1:10~1:50, is optimal with 1:30 especially.
In sum, the method for water-soluble multicolor carbon quantum point prepared by the microwave radiation of the present invention, completely at water
Carrying out in mutually, operate safety, fast and convenient, toxicity is little, and materials safety is easy to get.Can by accompanying drawing 1~accompanying drawing 6
To find out, the water-soluble multicolor carbon quantum point of gained has good monodispersity, photoluminescent property and quantum yield
Height, good stability, there is good water solublity, can as fluorescent marker be widely used in biological detection and
Analyze.
It is obvious to a person skilled in the art that the invention is not restricted to the details of above-mentioned one exemplary embodiment,
And without departing from the spirit or essential characteristics of the present invention, it is possible to realize in other specific forms
The present invention.Therefore, no matter from the point of view of which point, embodiment all should be regarded as exemplary, and right and wrong
Restrictive, the scope of the present invention is limited by claims rather than described above, it is intended that will fall
All changes in the implication of equivalency and scope of claim are included in the present invention.
Moreover, it will be appreciated that although this specification is been described by according to embodiment, but the most each enforcement
Mode only comprises an independent technical scheme, and this narrating mode of description is only for clarity sake,
Those skilled in the art should be using description as an entirety, and the technical scheme in each embodiment can also be through
Appropriately combined, form other embodiments that it will be appreciated by those skilled in the art that.
Claims (3)
1. the method that water-soluble multicolor carbon quantum point prepared by a microwave radiation, it is characterised in that include following
Step:
(1) organic carbon source and ultra-pure water being uniformly hybridly prepared into precursor solution standby, wherein, described has
Machine carbon source is milk, Mel, egg, Fructus Citri Limoniae juice or Magnolia denudata Desr.;
(2) precursor solution of gained is radiated at microwave power 15W~1000W, temperature 150 DEG C~180 DEG C
Heating 15min~300min, obtains water-soluble multicolor carbon quantum point.
Method the most according to claim 1, it is characterised in that: described organic carbon source is milk, its
With the mixed volume of ultra-pure water than for 1:10~1:50.
Method the most according to claim 2, it is characterised in that: described milk and the mixture of ultra-pure water
Long-pending ratio is 1:30.
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CN115247063B (en) * | 2021-04-27 | 2023-06-20 | 郑州大学 | Eggshell-based red carbon quantum dot and preparation method and application thereof |
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