CN104388082B - A kind of orange nitrogen, the green synthesis method of sulfur codope carbon quantum dot - Google Patents
A kind of orange nitrogen, the green synthesis method of sulfur codope carbon quantum dot Download PDFInfo
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- CN104388082B CN104388082B CN201410605756.9A CN201410605756A CN104388082B CN 104388082 B CN104388082 B CN 104388082B CN 201410605756 A CN201410605756 A CN 201410605756A CN 104388082 B CN104388082 B CN 104388082B
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Abstract
The invention discloses a kind of fluorescent orange nitrogen, sulfur is co-doped with the green synthesis method of carbon quantum dot.Described preparation method with two kinds of different aminoacid as raw material, water as solvent, realized by aminoacid polycondensation carburizing reagent under hydrothermal conditions.The present invention is simple to operate, raw material green, low cost, is easy to get, and product manufacturing cycle is short, and reproducible.The carbon quantum dot size uniform that prepared nitrogen, sulfur are co-doped with, can launch orange light, compensate for the vacancy that existing carbon quantum dot is launched at this wavelength, and product can be widely applied to bio-imaging, cell marking, the various fields such as false proof.
Description
Technical field
The present invention relates to the preparing technical field of nano-luminescent material, particularly relate to a kind of orange
Nitrogen, the green synthesis method of sulfur codope carbon quantum dot.
Background technology
Carbon quantum dot is to be purified carbon nanometer by the scientist of Clemson University of the U.S. in 2004
The novel nano structure material with carbon element found it is not intended to first during pipe.Sun et al. is in 2006
Year, laser ablation method successfully prepared carbon nano-particle at laboratory, and was officially named
" carbon quantum dot " (Carbon quantum dots is called for short CQDs).At present, the grinding of carbon quantum dot
Study carefully the focus just becoming luminescence generated by light field.
Carbon quantum dot has the following characteristics that its particle diameter is generally less than 10nm, is provided simultaneously with lower conversion
With upper conversion luminescent properties, light stability is fabulous, without photobleaching and optical flare, it is easy to surface work
The excellent specific property such as energyization, good biocompatibility, therefore can be widely used in cell/tissue labelling,
The fields such as pharmaceutical carrier, solaode and photocatalysis.
Carbon quantum dot can pass through laser ablation method, electrochemical process, arc discharge at present
Prepared by method, microwave method, combustion method etc..But there is instrument and equipment requirement height, system in these methods
Standby flow process is complicated, cost of material is high, it is difficult to scale, and products obtained therefrom size is uneven waits deficiency.
And the carbon quantum dot of current report mainly launches blueness, green, yellow.Long wavelength can be launched
The carbon quantum dot of (λ > 600nm), the carbon quantum dot that especially can launch fluorescent orange does not also have
Report.The existence of these problems all significantly limit the large-scale production of carbon quantum dot with extensive
Application.Therefore, develop a kind of green, scale simple, easy, the carbon amounts of long wavelength can be launched
The preparation method of son point has the using value of reality.
Summary of the invention
For the defect overcoming above-mentioned prior art to exist, it is an object of the invention to provide one
Nitrogen, sulfur are co-doped with the green synthesis method of carbon quantum dot.The method is simple to operate, environmental friendliness,
Low for equipment requirements, reproducible.Raw materials used is only aminoacid and water, and they prices are low
Honest and clean, wide material sources, green non-poisonous.And preparation nitrogen, the carbon quantum dot of sulfur codope have send out
The characteristic of orange light, can be widely used in bio-imaging, fluorescent probe, the field such as false proof.
To achieve the object of the present invention, the present invention adopts the following technical scheme that
The orange nitrogen of the present invention, the concrete steps of green synthesis method of sulfur codope carbon quantum dot
As follows:
(1) under agitation, CYSTINE and Serine are dissolved in pure water, before obtaining
The mol ratio driving liquid solution, CYSTINE and Serine is 1:0.5-2, CYSTINE and pure
The molal volume of water is than for 5:15-25mmol/ml；
(2) step (1) gained precursor solution is placed in reactor, in 160 DEG C-220 after sealing
React 2-8 hour at DEG C, after reaction terminates, be cooled to room temperature and obtain brownish red turbid solution；
(3) solution centrifugal step (2) obtained, obtains that can to launch the nitrogen of fluorescent orange, sulfur common
The carbon quantum dot product of doping.
In step (1), the preferably mol ratio of CYSTINE and Serine is 1:1.
In step (1), preferably the molal volume of CYSTINE and pure water is than for 5:20mmol/ml.
In step (2), preferable reaction temperature is 200 DEG C.
In step (2), the preferably response time is 5h.
In step (2), described reactor is the autoclave of teflon lined.
An object of the present invention also resides in provides a kind of preparation method of the present invention to prepare
Send out the nitrogen of orange light, the carbon quantum dot of sulfur codope.
The present invention compared with prior art has a following advantage:
1. the present invention is simple to operate, manufacturing cycle is short, needed raw material is green, simple and easy to get, institute
Method of stating is reproducible, can synthesize on a large scale；
2. prepared by the present invention send out the nitrogen of orange light, sulfur codope carbon quantum dot distribution of sizes equal
Even, avirulence, can be applicable to cell imaging field.
Accompanying drawing explanation
Fig. 1 is the transmission electron microscope of the N-S codope carbon quantum dot of the embodiment of the present invention 1 preparation
Figure.
Fig. 2 is the fluorescence spectrum of the N-S codope carbon quantum dot of the embodiment of the present invention 1 preparation
Figure.
Fig. 3 is that the N-S codope carbon quantum dot of the embodiment of the present invention 1 preparation is under variable concentrations
Process the survival rate block diagram of cell.
Fig. 4 is the transmission electron microscope of the N-S codope carbon quantum dot of the embodiment of the present invention 2 preparation
Figure.
Fig. 5 is the fluorescence spectrum of the N-S codope carbon quantum dot of the embodiment of the present invention 2 preparation
Figure.
Fig. 6 is the transmission electron microscope of the N-S codope carbon quantum dot of the embodiment of the present invention 3 preparation
Figure.
Fig. 7 is the fluorescence spectrum of the N-S codope carbon quantum dot of the embodiment of the present invention 3 preparation
Figure.
Fig. 8 is the transmission electron microscope of the N-S codope carbon quantum dot of the embodiment of the present invention 4 preparation
Figure.
Fig. 9 is the fluorescence spectrum of the N-S codope carbon quantum dot of the embodiment of the present invention 4 preparation
Figure.
Detailed description of the invention
For better illustrating the present invention, it is simple to understand technical scheme, below to this
Bright further description.But following embodiment is only the simple example of the present invention, and
Not representing or limit the scope of the present invention, protection scope of the present invention is with claim
Book is as the criterion.
Embodiment 1
(1) take 5mmol CYSTINE, 5mmol Serine is raw material, adds 20ml
Pure water, dissolves to obtain precursor solution after stirring.
(2) step (1) gained precursor solution is placed in reactor, 200 after sealing
React 5h at DEG C, be cooled to room temperature.
(3) solution centrifugal step (2) obtained, i.e. can get orange N-S codope
Carbon quantum dot.
Seeing accompanying drawing 1, it is the transmission electricity of the N-S codope carbon quantum dot of synthesis under the conditions of this
Mirror figure.As can be seen from the figure product is the carbon quantum dot of size uniform, size about 2.5 nanometer.
Seeing accompanying drawing 2, it is the fluorescence light of the N-S codope carbon quantum dot of synthesis under the conditions of this
Spectrogram.As can be seen from Figure 2 prepared carbon quantum dot is aobvious under 540nm excitation wavelength
Showing that hyperfluorescence is launched, emission peak is positioned at 610nm, is shown as orange light.
Seeing accompanying drawing 3, it is that the N-S codope carbon quantum dot prepared processes under variable concentrations
The survival rate block diagram of cell.Result shows that product shows negligible cytotoxicity.
Embodiment 2
(1) weigh 5mmol CYSTINE, 5mmol L-PROLINE respectively, add 20ml
Water, obtains precursor solution:
(2) step (1) gained precursor solution is placed in reactor, at 200 DEG C after sealing
Lower reaction 2h, is cooled to room temperature:
(3) solution centrifugal step (2) obtained, i.e. can get orange N-S codope
Carbon quantum dot:
Seeing accompanying drawing 4, it is the transmission electricity of the N-S codope carbon quantum dot of synthesis under the conditions of this
Mirror figure.Size about 6 nanometer of product can be measured from figure.The fluorescence spectrum chart of Fig. 5
Bright prepared carbon quantum dot shows that under 540nm excitation wavelength hyperfluorescence is launched, launches
Peak center is positioned at 607nm, for orange light.
Embodiment 3
(1) 5mmol CYSTINE, 5mmol ALANINE silk are dissolved in 20ml water,
Obtain precursor solution:
(2) step (1) gained precursor solution is placed in reactor, at 200 DEG C after sealing
Lower reaction 5h, is cooled to room temperature.
(3) solution centrifugal step (2) obtained, i.e. can get orange N-S codope
Carbon quantum dot.
Seeing accompanying drawing 6, it is the transmission electricity of the N-S codope carbon quantum dot of synthesis under the conditions of this
Mirror figure.Size about 8 nanometer of product can be measured from figure.The fluorescence spectrum chart of Fig. 7
Bright prepared carbon quantum dot shows that under 540nm excitation wavelength hyperfluorescence is launched, launches
Peak center is positioned at 604nm, for orange light.
Embodiment 4
(1) 5mmol CYSTINE, 5mmol altheine are dissolved in 20ml water,
Obtain precursor solution:
(2) step (1) gained precursor solution is placed in reactor, at 200 DEG C after sealing
Lower reaction 5h, is cooled to room temperature.
(3) solution centrifugal step (2) obtained, i.e. can get orange N-S codope
Carbon quantum dot.
Seeing accompanying drawing 8, it is the transmission electricity of the N-S codope carbon quantum dot of synthesis under the conditions of this
Mirror figure.Size about 13 nanometer of product can be measured from figure.The fluorescence spectrum figure of Fig. 9
Show that prepared carbon quantum dot shows that under 500nm excitation wavelength hyperfluorescence is launched, sends out
Penetrate peak center and be positioned at 593nm, for orange light.
Embodiment 5
Take the C57BL/6 mice in 6-8 week, in sterilizing room, with the ethanol solution pair of 75%
Mice carries out disinfection 5 minutes, by the serum-free DMEM culture fluid of 8mL (containing 10% tire
Ox blood serum, penicillin 100U/mL, streptomycin 100 μ g/mL) inject mice abdominal cavity,
4mL ascites is extracted out with syringe after 5 minutes.Then the cell putting it into 6 orifice plates is cultivated
In ware, it is 37 DEG C in temperature, cultivates in the incubator containing CO25%.After 12 hours
Change culture fluid, to remove a small amount of attached cell.The carbon quantum dot that nitrogen, sulfur are co-doped with is put into carefully
Born of the same parents' culture fluid is further cultured for 12 hours, observes with common inverted fluorescence microscope,
Can get the cell fluorescence image under green glow excites.Fluorescence microscope images shows, at green glow
Exciting down, cell can show obvious redness.This result shows nitrogen, the carbon amounts of sulfur codope
Son point can be applicable to cell marking.
Although an embodiment of the present invention has been shown and described, for the ordinary skill of this area
For personnel, it is possible to understand that without departing from the principles and spirit of the present invention can be to this
A little embodiments carry out multiple change, revise, replace and modification, and the scope of the present invention is by appended power
Profit requires and equivalent limits.
Claims (6)
1. an orange nitrogen, the green synthesis method of sulfur codope carbon quantum dot, it is characterised in that:
Specifically comprising the following steps that of described method
(1) under agitation, CYSTINE and Serine are dissolved in pure water, before obtaining
The mol ratio driving liquid solution, CYSTINE and Serine is 1:0.5-2, CYSTINE and pure
The molal volume of water is than for 5:15-25mmol/ml；
(2) step (1) gained precursor solution is placed in reactor, in 160 DEG C-220 after sealing
React 2-8 hour at DEG C, after reaction terminates, be cooled to room temperature and obtain brownish red turbid solution；
(3) solution centrifugal step (2) obtained, must launch the nitrogen of fluorescent orange, sulfur is co-doped with
Miscellaneous carbon quantum dot product.
Orange nitrogen the most as claimed in claim 1, the green synthesis method of sulfur codope carbon quantum dot,
It is characterized in that: in step (1), the mol ratio of CYSTINE and Serine is 1:1.
Orange nitrogen the most as claimed in claim 1, the green synthesis method of sulfur codope carbon quantum dot,
It is characterized in that: in step (1), the molal volume of CYSTINE and pure water is than for 5:20
mmol/ml。
Orange nitrogen the most as claimed in claim 1, the green synthesis method of sulfur codope carbon quantum dot,
It is characterized in that: in step (2), reaction temperature is 200 DEG C.
Orange nitrogen the most as claimed in claim 1, the green synthesis method of sulfur codope carbon quantum dot,
It is characterized in that: in step (2), the response time is 5h.
Orange nitrogen the most as claimed in claim 1, the green synthesis method of sulfur codope carbon quantum dot,
It is characterized in that: in step (2), described reactor is that the high pressure of teflon lined is anti-
Answer still.
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| CN104804734B (en) * | 2015-04-01 | 2017-04-19 | 河南师范大学 | Synthesis method for sulfur-nitrogen-doped fluorescent carbon dots according to one-step microwave method |
| CN105542760A (en) * | 2015-12-28 | 2016-05-04 | 江南大学 | Preparation method of nitrogen- and sulfur-doped fluorescence carbon dots |
| CN105419794B (en) * | 2015-12-30 | 2017-12-15 | 中国科学院长春光学精密机械与物理研究所 | A kind of orange light transmitting carbon nano dot and its preparation method and application |
| CN105838363B (en) * | 2016-04-21 | 2018-04-10 | 大连理工大学 | A kind of method based on amino acid and iron ion synthesis carbon quantum dot |
| CN106587007A (en) * | 2016-11-22 | 2017-04-26 | 上海纳米技术及应用国家工程研究中心有限公司 | Nitrogen-sulfur-doped pH-sensitive carbon quantum dots and preparing method and application |
| CN106904592B (en) * | 2017-02-27 | 2018-08-31 | 西南大学 | A kind of preparation method of fluorescent orange carbon quantum dot |
| CN107219210B (en) * | 2017-07-26 | 2019-04-26 | 广西师范学院 | Utilize the method for water-soluble fluorescent orange carbon quantum dot probe in detecting hemoglobin |
| CN108018039B (en) * | 2017-12-18 | 2020-08-25 | 河北工业大学 | Preparation method and application of white light emitting carbon quantum dots |
| CN109207149A (en) * | 2018-11-02 | 2019-01-15 | 山西大学 | A kind of nitrogen, sulphur codope yellow fluorescence carbon dots and its application in anticancer drug |
| CN109321240B (en) * | 2018-11-23 | 2020-06-09 | 江南大学 | Orange fluorescent carbon dot and preparation method thereof |
| CN109467074A (en) * | 2018-12-13 | 2019-03-15 | 南京师范大学 | A kind of carbon quantum dot and the preparation method and application thereof improving adriamycin anti-cancer effectiveness |
| CN110591705B (en) * | 2019-09-15 | 2022-07-12 | 浙江大学山东工业技术研究院 | Carbon quantum dot suitable for fluorescence immunochromatography labeling and preparation method thereof |
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| CN103086355A (en) * | 2013-02-01 | 2013-05-08 | 浙江大学 | Synthetic method of carbon quantum dot material |
| CN103693633A (en) * | 2013-12-04 | 2014-04-02 | 上海交通大学 | Method for green synthesis of fluorescent chiral carbon dots |
| CN104089999A (en) * | 2014-06-25 | 2014-10-08 | 复旦大学 | Carbon quantum dot-nanowire array-based cardiomyocyte signal molecule sensor and preparation method thereof |
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| CN103086355A (en) * | 2013-02-01 | 2013-05-08 | 浙江大学 | Synthetic method of carbon quantum dot material |
| CN103693633A (en) * | 2013-12-04 | 2014-04-02 | 上海交通大学 | Method for green synthesis of fluorescent chiral carbon dots |
| CN104089999A (en) * | 2014-06-25 | 2014-10-08 | 复旦大学 | Carbon quantum dot-nanowire array-based cardiomyocyte signal molecule sensor and preparation method thereof |
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