CN105905884A - Preparation method and application of fluorescence carbon quantum dots - Google Patents
Preparation method and application of fluorescence carbon quantum dots Download PDFInfo
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Abstract
The invention provides a preparation method and an application of fluorescence carbon quantum dots. The fluorescence carbon quantum dots with excellent optical performances are synthesized from natural spinach under hydrothermal conditions through a one-step technology. The fluorescence carbon quantum dots emit blue lights under an ultraviolet light source, the quantum efficiency of the fluorescence carbon quantum dots is 53%, the fluorescence carbon quantum dots can be stored for a long term without generating precipitates, the fluorescence is difficult to bleach, and can last for 6 or more months, and the fluorescence carbon quantum dots can be used as fluorescent ink. The preparation method of the fluorescence carbon quantum dots is a simple one-time green synthesis route without any surface passivating agents, so the method has the characteristics of low cost, simple synthesis process and easy operation. A method for using a carbon quantum dot solution prepared from spinach as the fluorescent ink is simple to operate and is environmentally-friendly, and the carbon quantum dots can be used as a fluorescence imaging material, and also can be used for cell fluorescence imaging.
Description
Technical field
The invention belongs to nano application technical field, be specifically related to synthetic method and the application of a kind of fluorescent carbon quantum dot.
Background technology
Nano-sized carbon point, also referred to as carbon quantum dot (C-Dots), be the class Novel Carbon Nanomaterials that is smaller in size than 10 nm,
Find first in time within 2004, purifying single-layer carbon nano-tube by electrophoresis method.Owing to its raw material resources is abundant and cheap and excellent
Different water solublity, chemical inertness, hypotoxicity, easy sense dough and anti-light bleaching power, carbon point is increasingly becoming carbon nanomaterial man
A nova in race.Carbon is typically considered a kind of black material, and fluorescence is more weak.And why carbon point can attract extensively
The reason of concern be that it has the strongest photoluminescent property, the most also referred to as fluorescent carbon point.It is understood that carbon is
In the earth and universe, content is compared with the element of horn of plenty, it is important that tellurian life all based on carbon, so
The nano material of carbon is compared with the nano material of other element, and much lower to the toxicity of organism, biological safety is the highest,
Substantially without bringing environmental problem.
In in recent years, oneself is through there being the synthetic method of a lot of quantum dot, and has in characteristic and the application aspect of quantum dot
The biggest progress.Owing to transmitting wavelength and the excitation wavelength spectrum of fluorescent carbon quantum dot are continuous and wide, can be by changing carbon point
Size carry out harmony and launch wavelength and excitation wavelength, there is the glimmering of the advantages such as the most anti-fast light Bleachability, stable chemical nature
Light characteristic it be widely used and analyzing multiple fields such as detection, photocatalysis, opto-electronic conversion, bio-imaging.With traditional half
Conductor quantum dot is compared with organic dyestuff, and fluorescent carbon point has more preferable water solublity, fast light Bleachability, low toxicity, biocompatibility
Etc..Therefore it can be used in the field such as biomarker, detection, such as [Hsu P C, Shih Z Y, Lee C such as Chang
H, et al. Synthesis and analytical applications of photoluminescent carbon
Nanodots [J]. Green Chem., 2012,14,917-920.] that the carbon quantum dot of preparation is acted on LLC-PK1 is thin
Born of the same parents, test its practicality for cell imaging.[Cao L, Wang X, M. Meziani J, the et al. such as Cao
Carbon dots for multiphoton bioimaging[J]. J.Am. Chem. Soc., 2007, 129,
11318-11319.] carbon quantum dot that PPEI-m is passivated is successfully applied to the cell imaging of Human Breast Cancer MCF-7 cell.System
The method of standby carbon quantum dot has a lot, such as [Zhou J Q Booker C, Li R Y, et such as electrochemical synthesis, Zhou
al. An electrochemical avenue to blue luminescent nanocrystals from
multiwalled carbon nanotubes (MWCNTs) [J], J. Am. Chem. Soc., 2007, 129 (4),
Pp 744 745] to choose tetrabutylammonium perchlorate acetonitrile solution be electrolyte solution, with CNT as electrode, the carbon prepared
Point sends blue-fluorescence, and fluorescence is relatively strong, and particle diameter about 2.8 nm ± 0.5 nm, fluorescence quantum yield is 6.4%.Laser disappears
Melt preparation method, [Haitao Li, Xiaodie He, Yang Liu, Hang Yu, Zhenhui Kang, the Shuit-such as Li
Tong Lee, Synfliesis of fluorescent carbon nanopartides direcdyfrm active
Caibon via a ultrasonic treatmait [J]. Mater. Res. Bull. 2011,46,147-151.] use
Ultrasonic method has processed nano-carbon powder, and the granule after then processing is put in common solvents, such as: water, ethanol.Will eventually get
Black suspension solution, it is not necessary to passivation agents directly with laser irradiate, obtain fluorescent carbon point.Hydrothermal synthesis method, [the Pan such as Pan
D,Zhang J. Li Z. et al. Hvdrotheimal route for cutting graphene sheets into
blue-luminescent graphene quantum dots [J]. Adv. Mater.. 2010, 22, 734-738.]
By in dilute for graphite oxide mixed solution joining NaOH and water, finally solution is put in reactor and heat, thus obtain energy
Sending the carbon quantum dot of blue-fluorescence, particle diameter is 5-13 nm, and its quantum yield is 6.9%.Also have template etc. a lot
Method, but these methods are not operation complexity needs material costly or instrument and the carbon quantum dot that obtains glimmering exactly
Photo-quantum efficiency is relatively low.The present invention introduces a kind of simple, and the efficient method synthesizing carbon quantum dot, simple to operate, raw material is just
Environmental protection is exactly with Herba Spinaciae as carbon source the most again, uses hydro-thermal method one step to add hot preparation carbon quantum dot.It should be noted that and the most only make
With pure water as solvent, it is not necessary to other acid, alkaline solution etc., the carbon point therefore prepared eliminates a lot of harsh experiment condition
With complicated experimentation, and loaded down with trivial details purification process.The quantum point grain diameter that this method obtains, at 2-6 nm, has very well
Single dispersibility and good water solublity, the light of 405 nm can be sent under the excited by visible light of 330 nm, fluorescent emission is strong
Degree is the strongest, and quantum yield is about 53%, dips carbon point and writes, and writing presents fluorescent characters clearly under ultraviolet source
Mark, can be used as fluorescent ink；Can also be used for cell imaging field.
Summary of the invention
It is an object of the invention to provide the preparation method and application of a kind of carbon quantum dot.Use natural Herba Spinaciae as former
Material, utilizes hydro-thermal method to prepare fluorescent carbon point, is applied as fluorescent ink by the fluorescent carbon point obtained, has effect clearly, and
Can preserve for a long time, fluorescent carbon quantum dot is also used as fluorescent marker for cell fluorescence imaging.
A kind of fluorescent carbon quantum dot preparation method, it is characterised in that comprise the following steps:
First 3-10 g Herba Spinaciae is smashed to pieces, put in autoclave after adding the deionized water mixing of 20-25 mL and be heated to
180 DEG C-200 DEG C continue 10-24 h, after question response terminates, naturally cool to room temperature, staticly settle, remove big residuals
After carry out being filtrated to get the purest carbon quantum dot solution with the filter membrane of 0.22 μm again.
Obtained carbon quantum dot presents blue emission under ultraviolet source, surveys its fluorescence spectrum, at the wavelength of 330 nm
Under excite, fluorescent carbon quantum dot has strong emission peak at 405 nm, and the fluorescent emission of obtained carbon quantum dot is with the change of concentration
Changing and change (as shown in Figure 1), figure A represents the fluorescence emission spectrum diluted respectively by solution after 5 to 60 times at Ex=360 nm
Figure, figure B represents the fluorescent emission spectrogram diluted by solution after 5 to 60 times at Ex=390 nm, and its fluorescence spectrum figure is all as
The reduction of concentration, fluorescence intensity presents the trend of first increases and then decreases, and figure C corresponds under daylight lamp and variable concentrations under uviol lamp
Carbon quantum dot solution thereon, from fluorescence photo it can be seen that carbon quantum dot presents strong blue emission (accompanying drawing 1).Described fluorescence
The particle diameter size of carbon quantum dot is 2-6 nm, and spacing of lattice is 0.34 nm (accompanying drawing 2), and (002) corresponding to graphite is brilliant
Face；The composition fully proving carbon nano-quantum point is carbon (accompanying drawing 2).
Carbon amounts point fluorescent emission peak position and intensity also have excitation wavelength dependency, i.e. along with the change of excitation wavelength,
Emission peak also occurs to change accordingly, and along with the change of intensity.Excitation wavelength is increased to 430 nm by 290 nm, launches
Wavelength gradually red shift, simultaneously intensity first increases and then decreases (accompanying drawing 3).The carbon quantum dot fluorescence quantum efficiency prepared by Herba Spinaciae is
53%, this is more somewhat higher than the fluorescence quantum yield of the carbon quantum dot reported before, records glimmering when excitation wavelength is 370 nm
Optical attenuation curve, the mean fluorecence life value that can be obtained carbon quantum dot by matching fluorescence decay curve is that 6.51 ns are (attached
Fig. 4)；
The application of fluorescent carbon quantum dot:
1, as fluorescent ink
The method of described synthesis fluorescent carbon quantum dot, can be used as preparing fluorescent ink, is applied to fluorescence inkjet printing, pen sailor
The aspect such as write.We write " HRBNU " as fluorescent ink, often with the carbon quantum dot solution prepared on the reagent paper do not have fluorescence
Shoot once every a period of time, find that the intensity of fluorescence does not occur significantly change (accompanying drawing 5).Then we are by carbon quantum
Point solution is drawn onto in pen and uses (as shown in Figure 6) as ink, and A B figure represents that ink is 1 with carbon quantum dot solution ratio:
After 8-1:15 mixing, use pen write put under fluorescent light with the photo under uviol lamp, C D figure be that use carbon quantum dot is molten
Liquid write as ink after under fluorescent light with the photo under uviol lamp.Further the carbon point ink of variable concentrations is loaded
In the print cartridge of ink-jet printer, and computer is connected with printer can carry out fluorescent printing.These characteristics show, prepared by Herba Spinaciae
Fluorescent carbon quantum dot can as novel fluorescent ink, be applied to the storage of information, encryption, false proof, illumination display, sensing
Deng multiple fields.And fluorescent ink based on carbon quantum dot has low cost, the feature such as method is simple, environmental protection, convenient
Large-scale production, has important market using value.
2, for cell fluorescence imaging
Cell is cultivated and cell toxicology experiment: lung carcinoma cell (A549) is when cell grows to 50-60%, and tested material processes, will
After cell after process cultivates 24 h, every hole adds 20 μ L MTT(5 mg/mL), hatch 4 h, abandoning supernatant, every hole for 37 DEG C
Adding 150 μ L DMSO, under room temperature, shaker vibrates 10 min, measures optical absorbance value (A value), mensuration with microplate reader readout instrument
Wavelength 570 nm, a length of 630 nm of reference wave, each experiment sets 8, multiple hole.Carbon quantum dot is utilized to carry out cytotoxicity analysis
(MTT) test, tests out carbon quantum dot and carries out the optium concentration of cell imaging, with concentration and people's pulmonary carcinoma of optimal carbon quantum dot
Cell (A549) co-culture of cells carries out fluorescence imaging experiments.
We can observe that variable concentrations (0,0.013,0.016,0.020,0.027,0.040 g/ according to Fig. 7 (A)
ML) carbon quantum dot and A549 cell cultivate 24 h, after completing to cultivate, carry out the survival ability test of A549 cell, and it is thin
The survival ability of born of the same parents is the strongest, illustrates that carbon quantum dot is relatively low to the toxicity of cell, compared with other biological probe, and carbon quantum dot
There is good cell compatibility, illustrate that this fluorescent carbon quantum dot avirulence, Fig. 7 (B) are that fluorescent carbon quantum dot is used as cell
The fluorogram of picture.
Beneficial effect:
1, the invention provides fluorescent carbon quantum dot preparation method, prepared fluorescent carbon quantum dot has strong blue emission, and
And can be used as fluorescent ink.
2, the present invention easily prepares and preserves；8 can be preserved under the conditions of 4 ° of C～do not change for 15 months.
3, agents useful for same of the present invention and operating process all have no side effect.
4, the inventive method simple, quickly, easily operation, practical.
Accompanying drawing explanation
Below in conjunction with the accompanying drawings and embodiment the present invention is further detailed explanation:
Accompanying drawing 1 is the fluorescence spectrum figure of variable concentrations carbon quantum dot；
Accompanying drawing 2 is the high resolution TEM photo of carbon quantum dot；
Accompanying drawing 3 is the emission spectrum figure of carbon quantum dot under different shooting condition；
Accompanying drawing 4 is fluorescence decline curve and the matched curve of fluorescent carbon quantum dot；
Accompanying drawing 5 is the fluorescent carbon quantum dot application as fluorescent ink, A B C D tetra-pictures respectively in December, 2015,
In January, 2016, in February, 2016, in March, 2016 shoot；
Accompanying drawing 6 is the fluorescent carbon quantum dot actual application as ink, and A B is respectively after mixed ink under fluorescent light and purple
Writing photo under outer lamp；C D be only with carbon quantum dot solution as ink under fluorescent light with the writing photo under uviol lamp；
Accompanying drawing 7(A) the 24 h bodies of carbon quantum dot of variable concentrations (0,0.013,0.016,0.020,0.027,0.040 g/mL)
The investigation of outer cell survival rate, uses A549 cell to be estimated the cytotoxicity of carbon quantum dot；(B) cell imaging fluorescence
Figure.
Detailed description of the invention
Below in conjunction with specific embodiment, the present invention is expanded on further.
1, a kind of preparation method based on carbon quantum dot fluorescent ink, it is characterised in that comprise the following steps:
First 3 g Herba Spinaciaes are smashed to pieces, put into after adding the deionized water mixing of 20 mL and autoclave carries out be heated to 180 DEG C hold
Continuous 10 h, after question response terminates, naturally cool to room temperature, staticly settle, and remove after big residuals again by the mistake of 0.22 μm
Filter membrane carries out being filtrated to get the purest carbon quantum dot solution.
2, a kind of preparation method based on carbon quantum dot fluorescent ink, it is characterised in that comprise the following steps:
First 10 g Herba Spinaciaes are smashed to pieces, put into after adding the deionized water mixing of 25 mL and autoclave carries out be heated to 200 DEG C hold
Continuous 24 h, after question response terminates, naturally cool to room temperature, staticly settle, and remove after big residuals again by the mistake of 0.22 μm
Filter membrane carries out being filtrated to get the purest carbon quantum dot solution.
Obtained carbon quantum dot presents blue emission under ultraviolet source, and its fluorescence spectrum is along with the reduction of concentration, glimmering
Light intensity is the trend (accompanying drawing 1) of first increases and then decreases, and the particle diameter size of described fluorescent carbon quantum dot is 2-6 nm, lattice
Spacing is 0.34 nm (accompanying drawing 2).
2, described synthesis fluorescent carbon quantum dot can be used as preparing fluorescent ink.We use the carbon quantum dot solution conduct prepared
Fluorescent ink is write " HRBNU " on the reagent paper do not have fluorescence, shoots once every other month, finds the intensity of fluorescence not
Weaken (accompanying drawing 5).Then carbon quantum dot solution is drawn onto in pen and uses (as shown in Figure 6), A, B as ink by we
After figure represents that ink and carbon quantum dot solution are than mix for 1:8-1:15, use pen write put under fluorescent light with uviol lamp
Under photo, C, D figure be placed on after carbon quantum dot solution writes as ink under fluorescent light with uviol lamp under shooting photo.
These characteristics show, fluorescent carbon quantum dot prepared by Herba Spinaciae can be applied to the storage of information as novel fluorescent ink, add
The multiple fields such as close, false proof, illumination display, sensing.
3, described synthesis fluorescent carbon quantum dot is used for cell fluorescence imaging
Cell is cultivated and cell toxicology experiment: lung carcinoma cell (A549) is when cell grows to 50-60%, and tested material processes, will
After cell after process cultivates 24 h, every hole adds 20 μ L MTT(5 mg/mL), hatch 4 h, abandoning supernatant, every hole for 37 DEG C
Adding 150 μ L DMSO, under room temperature, shaker vibrates 10 min, measures optical absorbance value (A value), mensuration with microplate reader readout instrument
Wavelength 570 nm, a length of 630 nm of reference wave, each experiment sets 8, multiple hole.Carbon quantum dot is utilized to carry out cytotoxicity analysis
(MTT) test, tests out carbon quantum dot and carries out the optium concentration of cell imaging, with concentration and people's pulmonary carcinoma of optimal carbon quantum dot
Cell (A549) co-culture of cells carries out fluorescence imaging experiments.
We can observe that variable concentrations (0,0.013,0.016,0.020,0.027,0.040 g/ according to Fig. 7 (A)
ML) carbon quantum dot and A549 cell cultivate 24 h, after completing to cultivate, carry out the survival ability test of A549 cell, and it is thin
The survival ability of born of the same parents is the strongest, illustrates that carbon quantum dot is relatively low to the toxicity of cell, compared with other biological probe, and carbon quantum dot
There is good cell compatibility.Fig. 7 (B) is the fluorogram of cell imaging.
Claims (2)
1. the preparation method of a fluorescent carbon quantum dot, it is characterised in that comprise the following steps:
3-10 g Herba Spinaciae is smashed to pieces, put into after adding the deionized water mixing of 20-25 mL autoclave is carried out be heated to 180 DEG C-
200 DEG C, continue 10-24 h, after question response terminates, naturally cool to room temperature, staticly settle, use again after removing big residuals
The filter membrane of 0.22 μm carries out being filtrated to get the purest carbon quantum dot solution.
2. the application of a fluorescent carbon quantum dot, it is characterised in that described fluorescent carbon quantum dot solution is used as fluorescent ink at reagent paper
On write, under ultraviolet source, present writing clearly, and can persistently preserve more than 12 months, be applied to information storage and
Encryption, additionally it is possible to as fluorescence imaging material, for cell fluorescence imaging.
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| CN106752380A (en) * | 2016-12-19 | 2017-05-31 | 武汉大学 | A kind of aqueous Fluorescent Falsification-resistant Ink based on graphene quantum dot |
| CN107033888A (en) * | 2017-05-23 | 2017-08-11 | 天津工业大学 | Chinese medicine dreg prepares carbon point and its research for Antiforge fluorescent ink |
| CN107057463A (en) * | 2016-12-19 | 2017-08-18 | 武汉大学 | A kind of aqueous Fluorescent Falsification-resistant Ink based on carbon quantum dot |
| CN107555416A (en) * | 2017-08-07 | 2018-01-09 | 河南师范大学 | The method of hydro-thermal method synthetic nitrogen doping fluorescent carbon point |
| CN108059147A (en) * | 2017-12-27 | 2018-05-22 | 重庆文理学院 | A kind of method for preparing carbon material using discarded sunflower |
| CN108083257A (en) * | 2017-12-28 | 2018-05-29 | 湖南科技大学 | A kind of method that fluorescent carbon point is prepared using chloroplaset as carbon source |
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| CN109568578A (en) * | 2018-11-22 | 2019-04-05 | 广西师范大学 | Natural biomass quantum dot and biomass quantum dot-copper nano-complex preparation method and applications |
| CN109777412A (en) * | 2019-03-21 | 2019-05-21 | 山西大学 | A kind of pair of transmitting fluorescent carbon point and its preparation method and application |
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| CN107033888A (en) * | 2017-05-23 | 2017-08-11 | 天津工业大学 | Chinese medicine dreg prepares carbon point and its research for Antiforge fluorescent ink |
| CN107555416A (en) * | 2017-08-07 | 2018-01-09 | 河南师范大学 | The method of hydro-thermal method synthetic nitrogen doping fluorescent carbon point |
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