CN106629658A - Preparation method of fluorescent carbon quantum dot - Google Patents
Preparation method of fluorescent carbon quantum dot Download PDFInfo
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- CN106629658A CN106629658A CN201611041975.4A CN201611041975A CN106629658A CN 106629658 A CN106629658 A CN 106629658A CN 201611041975 A CN201611041975 A CN 201611041975A CN 106629658 A CN106629658 A CN 106629658A
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- C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
- C09K11/08—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials
- C09K11/65—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing carbon
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- C01P2002/80—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70
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- C01P2002/80—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70
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- C01P2004/04—Particle morphology depicted by an image obtained by TEM, STEM, STM or AFM
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- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/64—Nanometer sized, i.e. from 1-100 nanometer
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Abstract
The invention discloses a method for preparing a fluorescent carbon quantum dot by using a simple hydrothermal reaction. According to the method for preparing the fluorescent carbon quantum dot by using a hydrothermal method, a used carbon source is abandoned coffee slag. According to a concrete preparation process, the coffee slag and deionized water with the mass ratio being (1 to 50) to (1 to 10) are sufficiently mixed, and are then put into a reaction kettle; the reaction temperature is 150 to 200 DEG C; the heat preservation is performed for 5 to 20h; after the reaction is completed, cooling is performed at room temperature; a mixture of the fluorescent carbon quantum dot and the unreacted coffee slag is obtained; after filtering, liquid supernatant is taken through centrifugation; a dispersion solution of the fluorescent carbon quantum dot is obtained. The method for preparing the fluorescent carbon quantum dot has the advantages that the raw materials are cheap; the process conditions are simple; the operation achieves the green and environment-friendly effects; the cost is low; the repeatability is high; the yield is high; the amplification mass production can be easily realized, and the like.
Description
Technical field
The present invention relates to a kind of preparation method of fluorescent carbon quantum dot, particularly a kind of to be prepared using simple hydro-thermal reaction
The method of fluorescent carbon quantum dot.
Background technology
Quantum dot has unique quantum confined effect, skin effect, small-size effect, and becomes nano materials research
Focus, as quasi-zero dimension nano material, is applied in optics, electricity device, bio-imaging, the biological fields such as medicine that carry.
Because traditional semiconductor-quantum-point (such as CdSe, PbTe, CdTe etc.) and organic dyestuff are present, preparation method is loaded down with trivial details, price is held high
It is expensive, not environmentally, the shortcomings of easily there is photobleaching, limit its application, therefore develop preferable nontoxic and replacing with similarity
It is very necessary for nano material and its simple efficient green preparation method.
Carbon quantum dot is a kind of important fluorescence carbon nanomaterial, also referred to as carbon point, carbon nano dot, carbon nano-crystal etc., is
Size below 10nm, be completely dispersed, a class New Type of Carbon nano-functional material of the intimate torispherical of geometry.Fluorescence carbon quantum
Point particle size is little, and good water solubility, it is easy to functionalization, resistance to photobleaching is nontoxic, and with good biocompatibility so as to
In the neck such as optical device, cell imaging, medicament transport, biological detection, photocatalysis, solar cell, photoelectricity device, environmental science
Domain has broad application prospects.
Preparing the method for carbon quantum dot mainly has two kinds, method and from bottom to top method from top to bottom.From top to bottom method is mainly wrapped
Arc discharge, laser ablation, electrochemical oxidation etc. are included, such method generally requires harsh experiment condition, high cost, operation is multiple
It is miscellaneous, and yield is relatively low.From bottom to top method mainly includes hydrothermal synthesis method, microwave method, supercritical ultrasonics technology etc., and its experiment condition is simple,
Yield is higher, is easy to amplify batch production.Hydro-thermal method of the prior art because its peculiar advantage it is relatively broad apply, but generally
Need to use strong acid, highly basic or toxic reagent.
Chinese invention patent application 016101309488 discloses one kind with pomegranate seed as carbon source one-step synthesis fluorescence carbon amounts
The method of son point, the patent be fresh pomegranate seed, ethylenediamine and deionized water are well mixed after respectively by microwave method and water
Hot method one-step synthesis fluorescent carbon quantum dot.The patented method does not use strong acid to aoxidize, also without complicated last handling process, operation
Simple, non-toxic big reagent, the carbon source for being used is cheap and easy to get, and the carbon quantum dot of synthesis has stronger fluorescence, no
Bio-sensing is can be only used for, the fields such as cell imaging are can be also used for.
Cheap and easy to get, Nantural non-toxic, eco-friendly raw material are found as carbon source, for preparing carbon quantum dot, while keeping away
Exempt to introduce strong acid, highly basic, toxic reagent in preparation process, be that this area needs to solve a problem, and carbon quantum dot is green
It is also very important that color prepares the biologic applications to its later stage.
The content of the invention
The present invention provide it is a kind of overcome prior art it is not enough, do not use with hydro-thermal method preparation and in preparation process and appoint
The preparation method of the fluorescent carbon quantum dot of what strong acid, highly basic or toxic reagent.
It is discarded coffee grounds that the hydro-thermal method of the present invention prepares the carbon source used by the method for carbon quantum dot.
It by mass ratio is 1 that more specifically a kind of preparation process of the present invention is:50-1:10 coffee grounds fills with deionized water
Divide and reactor is put into after mixing, reaction temperature is 150-200 DEG C, is incubated 5-20h, is cooled down at room temperature after the completion of reaction, is obtained
To fluorescent carbon quantum dot and the mixture of unreacted coffee grounds, after filtration, centrifuging and taking supernatant obtains final product fluorescent carbon quantum dot
Dispersion liquid.
The dispersion liquid of the carbon quantum dot that the method for the present invention is prepared is dried by evaporation process, you can obtain carbon quantum
The dry powder of point.
The method for preparing fluorescent carbon quantum dot of the present invention has that raw material is cheap, process conditions simple, the green ring of operation
Guarantor, low cost, repeatability are by force, yield is big, be easy to the advantages of amplifying mass production.The fluorescent carbon quantum dot particle prepared
Size is tiny, be completely dispersed soilless sticking, fluorescence is strong.Due to its good biocompatibility and fluorescent characteristic, in optical device, cell
The fields such as imaging, medicament transport, biological detection, photocatalysis, solar cell, photoelectricity device, environmental science have using front
Scape.
Description of the drawings
Fig. 1 is transmission electron microscope (TEM) light field of the carbon quantum dot Jing after hydro-thermal reaction, filtration, centrifugation in embodiment 1
As figure.
Fig. 2 is transmission electron microscope (TEM) light field of the carbon quantum dot Jing after hydro-thermal reaction, filtration, centrifugation in embodiment 2
As figure.
Fig. 3 is that the photoelectron of the carbon quantum dot dry powder Jing after hydro-thermal reaction, filtration, centrifugation in embodiment 2 can (XPS) spectrum.
Fig. 4 is that imaging of the carbon quantum dot dispersion liquid to Hela cells is shone Jing after hydro-thermal reaction, filtration, centrifugation in embodiment 2
Piece.Left photo is the bright field image photo of Hela cells；Right photograph is photo of the Hela cells in the case where 403nm is excited.
Fig. 5 be embodiment 3 in Jing hydro-thermal reaction, filtrations, be centrifuged after carbon quantum dot dispersion liquid in the case where 650nm-900nm is excited
Up-conversion fluorescence spectrum.
Fig. 6 is the X-ray diffraction (XRD) of the carbon quantum dot granular powder Jing after hydro-thermal reaction, filtration, centrifugation in embodiment 4
Spectrum.
Fig. 7 is infrared light (FTIR) spectrum of the carbon quantum dot granular powder Jing after hydro-thermal reaction, filtration, centrifugation in embodiment 4.
Fig. 8 be embodiment 3 in Jing hydro-thermal reaction, filtrations, be centrifuged after carbon quantum dot dispersion liquid in the case where 340nm-480nm is excited
Down-conversion fluorescent spectrum.
Specific embodiment
The present invention is further elaborated with reference to embodiment.
Embodiment 1
The coffee grounds for reclaiming is dried, 1g coffee grounds is weighed and is added 50ml deionized waters, ultrasonic mixing 2h, after by mixture
The ptfe autoclave of 50ml is inserted, at 170 DEG C 5h is reacted.Reactor is cooled down at room temperature, filter paper mistake is used after cooling
Filter, after 5min is centrifuged under the conditions of 15000rpm, take supernatant liquid, obtain final product fully decentralized carbon quantum dot dispersion liquid, disperse
Liquid is in golden yellow.Deep in concentration Jing after evaporation, color is in dark-brown.
As shown in Fig. 1 TEM photos, made carbon quantum dot is completely dispersed, soilless sticking, and shape is in spherical, particle size
26.5-73.3nm, average particle size particle size 44.0nm.
Embodiment 2
The coffee grounds for reclaiming is dried, 3g coffee grounds is weighed and is added 50ml deionized waters, ultrasonic mixing 2h, after by mixture
The ptfe autoclave of 50ml is inserted, at 190 DEG C 5h is reacted.Reactor is cooled down at room temperature, filter paper mistake is used after cooling
Filter, after 5min is centrifuged under the conditions of 15000rpm, take supernatant liquid, obtain final product fully decentralized carbon quantum dot dispersion liquid, disperse
Liquid is in golden yellow.Deep in concentration Jing after evaporation, color is in dark-brown.
As shown in Fig. 2 TEM photos, made carbon quantum dot is completely dispersed, soilless sticking, and shape is in spherical, particle size
1.1-4.4nm, average particle size particle size 2.8nm.The dispersion liquid of a certain amount of carbon quantum dot is taken, in 80 DEG C of evaporation dryings.If Fig. 3 is carbon
, there is C, H, O, N peak in the XPS spectrum of quantum dot granular powder, side light carbon quantum dot surface has abundant hydroxyl, carboxylic in spectrum
The oxygen-containing functional groups such as base.Prepared carbon quantum dot can be used for Hela cell imagings, as shown in figure 4, left figure is Hela cells
Bright field image photo, it can be clearly seen that complete wedge shape cell outline.Fig. 4 right figures are photo of the cell in the case where 403nm is excited,
Can see that cell still has the profile consistent with bright field image, and cell is presented blue, illustrates the carbon quantum dot quilt for preparing
Cell swallows, and carbon quantum dot successfully marked cell.
Embodiment 3
The coffee grounds for reclaiming is dried, 3g coffee grounds is weighed and is added 50ml deionized waters, ultrasonic mixing 2h, after by mixture
The ptfe autoclave of 50ml is inserted, at 190 DEG C 10h is reacted.Reactor is cooled down at room temperature, filter paper mistake is used after cooling
Filter, after 5min is centrifuged under the conditions of 15000rpm, take supernatant liquid, obtain final product fully decentralized carbon quantum dot dispersion liquid, disperse
Liquid is in golden yellow.Deep in concentration Jing after evaporation, color is in dark-brown.
Made carbon quantum dot is completely dispersed, soilless sticking, and shape is in spherical, particle size 2.2-4.6nm, average grain chi
Very little 3.4nm.As shown in figure 5, prepared carbon quantum dot dispersion liquid is in the case where 650-900nm is excited, has in visible light wave range and substantially send out
Penetrate peak.Transmitting peak position increases with excitation wave wavelength, and red shift occurs, and shows as depending on the down-conversion fluorescent property for exciting.
Embodiment 4
The coffee grounds for reclaiming is dried, 5g coffee grounds is weighed and is added 50ml deionized waters, ultrasonic mixing 2h, after by mixture
The ptfe autoclave of 50ml is inserted, at 200 DEG C 10h is reacted.Reactor is cooled down at room temperature, filter paper mistake is used after cooling
Filter, after 5min is centrifuged under the conditions of 15000rpm, take supernatant liquid, obtain final product fully decentralized carbon quantum dot dispersion liquid, disperse
Liquid is in golden yellow.Deep in concentration Jing after evaporation, color is in dark-brown.
Made carbon quantum dot is completely dispersed, soilless sticking, and shape is in spherical, particle size 1.6-5.4nm, average grain chi
Very little 3.2nm.By carbon quantum dot dispersant liquid drop on silicon chip, it is to be dried after measure carbon quantum dot granular powder XRD spectrum, such as Fig. 6
It is shown, there is an amorphous bag near 24 °, illustrate that prepared carbon quantum dot is amorphous particle.Take dividing for a certain amount of carbon quantum dot
Dispersion liquid, in 80 DEG C of evaporation dryings.If Fig. 7 is the FTIR spectrums of carbon quantum dot granular powder, as shown in spectrum, carbon quantum dot contains abundant
Oxygen-containing functional group.As illustrated, prepared carbon quantum dot dispersion liquid has bright in the case where 340-480nm is excited in visible light wave range
Aobvious emission peak.Transmitting peak position increases with excitation wavelength, and red shift occurs, and shows as depending on the down-conversion fluorescent property for exciting.
Claims (3)
1. a kind of preparation method of fluorescent carbon quantum dot, is prepared using hydro-thermal method, it is characterised in that carbon source used is discarded coffee
Coffee slag.
2. the preparation method of fluorescent carbon quantum dot according to claim 1, it is characterised in that it by mass ratio is 1 to be:50-1:
10 coffee grounds puts into reactor after being sufficiently mixed with deionized water, reaction temperature is 150-200 DEG C, is incubated 5-20h, reaction
After the completion of cool down at room temperature, the mixture of fluorescent carbon quantum dot and unreacted coffee grounds is obtained, after filtration, in centrifuging and taking
Clear liquid, obtains final product the dispersion liquid of fluorescent carbon quantum dot.
3. the preparation method of fluorescent carbon quantum dot according to claim 2, it is characterised in that resulting carbon quantum dot
Dispersion liquid is dried by evaporation and processes the dry powder that carbon quantum dot is obtained.
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109054821A (en) * | 2018-07-13 | 2018-12-21 | 山西大学 | A kind of fluorescent carbon point and its preparation method and application |
| CN109879272A (en) * | 2019-04-16 | 2019-06-14 | 云南大学 | A method of multicolor fluorescence carbon quantum dot is prepared with tobacco wastewater |
| CN110104629A (en) * | 2019-05-20 | 2019-08-09 | 河南师范大学 | The method for synthesizing fluorescent carbon point as raw material one step hydro thermal method using wild gleditsia sinensis |
| CN113376128A (en) * | 2020-11-18 | 2021-09-10 | 成都理工大学 | Method for detecting sodium cyclamate by using coffee grounds fluorescent carbon quantum dots |
| CN114350352A (en) * | 2021-12-21 | 2022-04-15 | 广东药科大学 | Novel carbon material based on coffee beans and method for detecting lead ions and PPi |
| CN115125001A (en) * | 2022-08-23 | 2022-09-30 | 济南大学 | Preparation method of green luminescent carbon dots |
| CN115744878A (en) * | 2022-11-14 | 2023-03-07 | 兰州大学 | Fluorescent coffee grounds carbon quantum dots and preparation method and application thereof |
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Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109054821A (en) * | 2018-07-13 | 2018-12-21 | 山西大学 | A kind of fluorescent carbon point and its preparation method and application |
| CN109054821B (en) * | 2018-07-13 | 2021-05-14 | 山西大学 | Fluorescent carbon dot and preparation method and application thereof |
| CN109879272A (en) * | 2019-04-16 | 2019-06-14 | 云南大学 | A method of multicolor fluorescence carbon quantum dot is prepared with tobacco wastewater |
| CN109879272B (en) * | 2019-04-16 | 2022-07-15 | 云南大学 | Method for preparing multicolor fluorescent carbon quantum dots by using tobacco wastewater |
| CN110104629A (en) * | 2019-05-20 | 2019-08-09 | 河南师范大学 | The method for synthesizing fluorescent carbon point as raw material one step hydro thermal method using wild gleditsia sinensis |
| CN113376128A (en) * | 2020-11-18 | 2021-09-10 | 成都理工大学 | Method for detecting sodium cyclamate by using coffee grounds fluorescent carbon quantum dots |
| CN114350352A (en) * | 2021-12-21 | 2022-04-15 | 广东药科大学 | Novel carbon material based on coffee beans and method for detecting lead ions and PPi |
| CN114350352B (en) * | 2021-12-21 | 2023-09-08 | 广东药科大学 | Novel carbon material based on coffee beans and method for detecting lead ions and PPi |
| CN115125001A (en) * | 2022-08-23 | 2022-09-30 | 济南大学 | Preparation method of green luminescent carbon dots |
| CN115125001B (en) * | 2022-08-23 | 2023-04-28 | 济南大学 | Preparation method of green luminous carbon dots |
| CN115744878A (en) * | 2022-11-14 | 2023-03-07 | 兰州大学 | Fluorescent coffee grounds carbon quantum dots and preparation method and application thereof |
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