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 PDF

Info

Publication number
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
Authority
CN
China
Prior art keywords
water
carbon quantum
quantum point
microwave radiation
soluble
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Active
Application number
CN201310308250.7A
Other languages
Chinese (zh)
Other versions
CN103387219A (en
Inventor
何耀
汪婕
钟旖菱
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Suzhou University
Original Assignee
Suzhou University
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Suzhou University filed Critical Suzhou University
Priority to CN201310308250.7A priority Critical patent/CN103387219B/en
Publication of CN103387219A publication Critical patent/CN103387219A/en
Application granted granted Critical
Publication of CN103387219B publication Critical patent/CN103387219B/en
Active legal-status Critical Current
Anticipated expiration legal-status Critical

Links

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

The method of water-soluble multicolor carbon quantum point prepared by a kind of microwave radiation
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.
CN201310308250.7A 2013-07-22 2013-07-22 The method of water-soluble multicolor carbon quantum point prepared by a kind of microwave radiation Active CN103387219B (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201310308250.7A CN103387219B (en) 2013-07-22 2013-07-22 The method of water-soluble multicolor carbon quantum point prepared by a kind of microwave radiation

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201310308250.7A CN103387219B (en) 2013-07-22 2013-07-22 The method of water-soluble multicolor carbon quantum point prepared by a kind of microwave radiation

Publications (2)

Publication Number Publication Date
CN103387219A CN103387219A (en) 2013-11-13
CN103387219B true CN103387219B (en) 2016-08-10

Family

ID=49531656

Family Applications (1)

Application Number Title Priority Date Filing Date
CN201310308250.7A Active CN103387219B (en) 2013-07-22 2013-07-22 The method of water-soluble multicolor carbon quantum point prepared by a kind of microwave radiation

Country Status (1)

Country Link
CN (1) CN103387219B (en)

Families Citing this family (24)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103787299A (en) * 2014-01-02 2014-05-14 南京航空航天大学 Method for preparing high-brightness fluorescent carbon dots with single organic solvent by hot reflux method
CN103771390B (en) * 2014-01-06 2016-06-01 上海交通大学 The method of the auxiliary microwave method synthesis carbon quantum dot of a kind of bioactive enzyme, the carbon quantum dot thus prepared and application thereof
CN103803528B (en) * 2014-02-18 2016-04-13 南京瑞盈环保科技有限公司 The polyhedral preparation method of a kind of carbon
CN104030269B (en) * 2014-06-16 2015-12-30 广西师范大学 The preparation method of red carbon quantum dot and application
CN104192827A (en) * 2014-08-26 2014-12-10 上海交通大学 Method for synthesizing carbon quantum dots on basis of organic micromolecule microwave solid-phase reaction
CN104560036B (en) * 2014-12-30 2017-01-18 中国农业科学院农产品加工研究所 Carbon quantum dot fluorescence-labeled material adopting honey as carbon source, as well as preparation method and application thereof
CN105018082A (en) * 2015-07-10 2015-11-04 上海纳米技术及应用国家工程研究中心有限公司 Method for preparing carbon quantum dot labeled probe for silk fibroin extracted cell development
CN105293471B (en) * 2015-11-20 2017-12-08 武汉理工大学 A kind of method of carbon point/gelatin-compounded thing with sol-gel transition performance prepared by in-situ method
CN105502338A (en) * 2015-12-28 2016-04-20 江南大学 Method for microwave preparation of fluorescent carbon dots with green onion as raw material
CN106244142B (en) * 2016-07-25 2018-09-21 南京工业大学 A kind of preparation method of fluorescent carbon quantum dot polymer hybrid material
CN106318390B (en) * 2016-08-19 2019-01-04 北京化工大学 A kind of preparation method of biomass N doping fluorescent carbon point
CN106521548A (en) * 2016-11-10 2017-03-22 复旦大学 Electrocatalyst for sunlight-drive water electrolysis oxygen evolution reaction and preparation method of electrocatalyst
CN106629664B (en) * 2016-12-27 2018-12-04 江南大学 A kind of method and its application synthesizing carbon quantum dot using water chestnut as raw material microwave
CN107163935A (en) * 2017-06-13 2017-09-15 温州大学 A kind of method for synthesizing full light carbon point and its carbon point application
CN107523295A (en) * 2017-08-29 2017-12-29 湖南农业大学 A kind of fluorescent carbon point for the method and its preparation for preparing fluorescent carbon point as raw material using common flos traditional Chinese medicine material
CN109467072B (en) * 2017-09-07 2020-06-26 中国科学院福建物质结构研究所 Preparation method of carbon quantum dot, carbon quantum dot and MOFs composite film, product and application thereof
CN109705856A (en) * 2017-10-25 2019-05-03 哈尔滨工业大学 A method of fluorescent carbon quantum dot is prepared by predecessor microwave method of egg
CN109046328B (en) * 2018-06-25 2021-07-27 浙江工业大学 Photo-thermal catalytic hydrogenation catalyst, preparation thereof and application thereof in 3, 4-dichloronitrobenzene selective hydrogenation reaction
CN109046332B (en) * 2018-06-25 2021-08-24 浙江工业大学 Photo-thermal catalytic hydrogenation catalyst, and preparation method and application thereof
CN109046334B (en) * 2018-06-25 2021-07-27 浙江工业大学 Photo-thermal catalytic hydrogenation catalyst, preparation thereof and application thereof in p-benzoquinone selective hydrogenation reaction
CN109486486B (en) * 2018-12-21 2021-12-17 达州职业技术学院 Preparation method of fluorescent carbon quantum dots based on microwave method
CN110041925A (en) * 2019-05-21 2019-07-23 马娇 A kind of preparation method and applications of nitrogen sulfur doping carbon quantum dot
CN112010286A (en) * 2020-08-24 2020-12-01 江南大学 Method for preparing carbon quantum dots from milk
CN115247063B (en) * 2021-04-27 2023-06-20 郑州大学 Eggshell-based red carbon quantum dot and preparation method and application thereof

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101486905A (en) * 2008-08-28 2009-07-22 杭州大明荧光材料有限公司 Method for preparing blue fluorescent powder for PDP by high temperature microwave method
CN103086356A (en) * 2013-02-19 2013-05-08 复旦大学 Method for preparing carbon quantum dots
CN103172051A (en) * 2013-04-16 2013-06-26 苏州大学 Water-soluble carbon quantum dot and preparation method thereof

Family Cites Families (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102190296B (en) * 2011-06-15 2015-07-15 昆明物理研究所 Hydrothermal method for preparing water-soluble graphene quantum dots

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101486905A (en) * 2008-08-28 2009-07-22 杭州大明荧光材料有限公司 Method for preparing blue fluorescent powder for PDP by high temperature microwave method
CN103086356A (en) * 2013-02-19 2013-05-08 复旦大学 Method for preparing carbon quantum dots
CN103172051A (en) * 2013-04-16 2013-06-26 苏州大学 Water-soluble carbon quantum dot and preparation method thereof

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
Microwave synthesis of fluorescent carbon nanoparticles with electrochemiluminescence properties;Hui Zhu et.al.;《chemical communications》;20090716;5118-5120 *

Also Published As

Publication number Publication date
CN103387219A (en) 2013-11-13

Similar Documents

Publication Publication Date Title
CN103387219B (en) The method of water-soluble multicolor carbon quantum point prepared by a kind of microwave radiation
Guo et al. Tunable multicolor carbon dots prepared from well-defined polythiophene derivatives and their emission mechanism
Hola et al. Graphitic nitrogen triggers red fluorescence in carbon dots
Wisser et al. Enhancing quantum yield via local symmetry distortion in lanthanide-based upconverting nanoparticles
Liu et al. Surface sensitive photoluminescence of carbon nanodots: coupling between the carbonyl group and π-electron system
Zhang et al. Highly photoluminescent carbon dots derived from egg white: facile and green synthesis, photoluminescence properties, and multiple applications
CN104449693B (en) The preparation method of the fluorescent carbon quantum dot of nitrogen sulfur doping
Liu et al. One-pot synthesis of ternary CuInS 2 quantum dots with near-infrared fluorescence in aqueous solution
Fang et al. Easy synthesis and imaging applications of cross-linked green fluorescent hollow carbon nanoparticles
Wang et al. Highly luminescent organosilane‐functionalized carbon dots
Zhao et al. High-quality carbon nitride quantum dots on photoluminescence: effect of carbon sources
CN104528692A (en) Synthesis method of nitrogen-doped fluorescent carbon dots
Aiyer et al. Fluorescent carbon nanodots for targeted in vitro cancer cell imaging
CN105199717B (en) 2 mercaptoimidazole bovine serum albumin(BSA) fluorescent au nanocluster materials and preparation method thereof
CN106753353A (en) A kind of orange light and near infrared emission polymer carbon nano dot and preparation method thereof
CN105647526A (en) Near-full-spectrum fluorescent nanocarbon dots and preparation method thereof
CN104477900A (en) Method for preparing multicolor fluorescent graphene quantum dots by microwave process
Zhang et al. Recent advances in graphene quantum dots as bioimaging probes
CN106629664B (en) A kind of method and its application synthesizing carbon quantum dot using water chestnut as raw material microwave
Wei et al. ZnO: Er, Yb, Gd particles designed for magnetic-fluorescent imaging and near-infrared light triggered photodynamic therapy
CN104555978B (en) The preparation method of a kind of photoluminescence carbon quantum dot
CN105032462B (en) A kind of preparation method of iron nitrogen-doped carbon nano particle photocatalyst
CN108559496A (en) A method of preparing green fluorescence carbon quantum dot
He et al. Multifunctional carbon dots with solid–liquid state orange light emission for vitamin b12 sensing, cellular imaging, and red/white light-emitting diodes
CN103980904B (en) A kind of lithium yttrium fluoride nano composite material and preparation method thereof and the application in photodynamic therapy

Legal Events

Date Code Title Description
C06 Publication
PB01 Publication
C10 Entry into substantive examination
SE01 Entry into force of request for substantive examination
C14 Grant of patent or utility model
GR01 Patent grant
CP02 Change in the address of a patent holder

Address after: Suzhou City, Jiangsu province 215123 Xiangcheng District Ji Road No. 8

Patentee after: Soochow University

Address before: 215123 Suzhou Industrial Park, Jiangsu Road, No. 199

Patentee before: Soochow University

CP02 Change in the address of a patent holder