CN108083258A - A kind of double emission peak carbon quantum dots of concentration-dependant and preparation method - Google Patents
A kind of double emission peak carbon quantum dots of concentration-dependant and preparation method Download PDFInfo
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- CN108083258A CN108083258A CN201711499813.XA CN201711499813A CN108083258A CN 108083258 A CN108083258 A CN 108083258A CN 201711499813 A CN201711499813 A CN 201711499813A CN 108083258 A CN108083258 A CN 108083258A
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Abstract
The present invention provides a kind of double emission peak carbon quantum dot of concentration-dependant and preparation method, belong to the preparation field of nano material.Preparation method of the present invention is using citric acid as carbon source, using glycine as nitrogen source, has synthesized double emission peak carbon quantums with concentration dependant characteristic through one step hydro thermal method, can adjust the different double transmitting fluorescent characteristics of carbon quantum dot by concentration.Experimental raw is simple and easy to get, environmentally safe pollution-free, is conducive to carbon quantum dot and further applies photoelectric device, biosensor etc..
Description
Technical field
A kind of double emission peak carbon quantum dots of concentration-dependant of the present invention and preparation method belong to the preparation neck of nano material
Domain.
Background technology
Carbon dots (carbon dots, C-Dots) is a kind of new carbon after fullerene, carbon nanotubes and graphene
Nano material, shape approximation ball-type, size are generally less than 10 nanometers of nanocrystal.The core of carbon dots is generally by Sp2 hybridized nanometers
Brilliant carbon or amorphous carbon composition, spacing of lattice are consistent with the spacing of lattice of graphite or amorphous carbon.On carbon dots surface, there are energy
Potential well, after surface modification, the raising of fluorescence quantum yield is attributable to the variation of the surface state of carbon dots；Dimensional effect
Also play the role of to the fluorescence property of carbon dots very big.
As a kind of potential nano-substance to play a significant role in numerous areas, the excellent photoluminescent property of carbon dots is main
Have：Excitation wavelength scope is wide and continuous；Fluorescent stability is high and anti-light bleaching；Carbon dots is excellent electron donor and receptor,
With Photo-induced electron transfer characteristic.This nano material also has good biocompatibility, it is easy to accomplish and it is surface-functionalized,
There is good application potential in fields such as biochemical sensitive, imaging analysis, environment measuring, photocatalysis technology and pharmaceutical carriers.And
It can realize that Color tunable becomes application by adjusting strength of doublet with double emission peak carbon quantum dot materials.
At present, fluorescence carbon quantum is mostly monochromatic luminous, and the synthesis side of the carbon quantum dot for the adjustable fluorescent emission of polychrome
Method is but seldom reported.104927849 A of Chinese patent CN disclose a kind of high-fluorescence quantum yield blue-fluorescence carbon quantum dot
Green synthesis method.This method synthesizes carbon quantum dot using citric acid and glycine as raw material, using pyrolysismethod, and through organic molten
Agent extraction obtains the carbon quantum dot of high-fluorescence quantum yield.Carbon quantum dot prepared by this method water-soluble solution or can be both dissolved in
Polar organic solvent, however carbon quantum dot prepared by this method does not have double emission peak fluorescent characteristics.
It is contemplated that with double emission peak carbon quantum dots in terms of imaging analysis and environment measuring with very important application,
Therefore the more simple, fast double transmitting carbon quantum dots of research have vast potential for future development.
The content of the invention
The object of the present invention is to provide a kind of double emission peak carbon quantum dots of concentration-dependant and preparation method, this method systems
Standby carbon quantum dot has different Two peak emission fluorescent characteristics under different concentration.
Technical scheme is as follows：
A kind of double emission peak carbon quantum dots of concentration-dependant and preparation method, it is characterised in that include the following steps：
(1) citric acid and glycine are dissolved in certain proportion in a certain amount of pure water, magnetic agitation 10min makes it mixed
It closes uniformly, forms transparent mixed solution.
(2) transparent mixed solution in step (1) is taken to be transferred in the stainless steel autoclave of polytetrafluoroethyllining lining
Hydro-thermal reaction is carried out, is cooled to room temperature after hydro-thermal reaction.
(3) product obtained in step (2) is first removed into large granular impurity through centrifugation, then it is miscellaneous through filter membrane removal little particle
Matter obtains brown filtrate.
(4) the brown filtrate obtained in step (3) addition pure water is made into the carbon quantum dot solution of various concentration.
The molar ratio of citric acid and glycine is 1 in the step (1): (0.25~1), the volume of pure water used in dissolving
For 10ml.
Hydrothermal temperature is 150 DEG C~180 DEG C in the step (2), and the reaction time is 3~12h.
Centrifugal rotational speed is 10000rpm, centrifugation time 15min in the step (3)；Filter membrane is 0.22 micron of aperture
Filter membrane.
Carbon quantum dot concentration in the step (4) is followed successively by 10mg/ml, 3mg/ml, 2mg/ml, 1mg/ml.
The present invention has following features：
1. the present invention, using glycine as nitrogen source, can be synthesized directly using citric acid as carbon source by one step hydro thermal method
The double emission peak carbon dotss of concentration-dependant, preparation process is succinctly, conveniently.
It is a kind of green syt route 2. raw material of the present invention are simple and easy to get, cheap, environmentally safe pollution-free.
3. the carbon quantum dot that the present invention synthesizes can realize different Two peak emission fluorescent characteristics by regulating and controlling concentration, have
It is widely applied in environment measuring and imaging analysis etc. beneficial to carbon quantum dot.
Description of the drawings
Fig. 1 is fluorescence emission spectrum of the various concentration carbon dots sample under 365nm excitation wavelengths, and (a) concentration is 10mg/ml
Carbon dots sample, (b) concentration be 3mg/ml carbon dots sample, (c) concentration be 2mg/ml carbon dots sample, (d) concentration be 1mg/
The carbon dots sample of ml.
Fig. 2 is the UV absorption picture of various concentration carbon dots sample, and (a) concentration is the carbon dots sample of 10mg/ml, and (b) is dense
The carbon dots sample for 3mg/ml is spent, (c) concentration is the carbon dots sample of 2mg/ml, and (d) concentration is the carbon dots sample of 1mg/ml.
Fig. 3 is Fourier's infrared analysis picture of carbon dots sample.
Fig. 4 is X-ray diffraction (XRD) picture of carbon dots sample.
Specific embodiment
Below in conjunction with the drawings and specific embodiments, the invention will be further described.
Embodiment 1：
It weighs 1g citric acids and 0.391g glycine (molar ratio 1: 1) is dissolved in the pure water of 10ml, magnetic agitation
10min is allowed to be formed uniformly transparent mixed solution, and mixed solution is transferred to polytetrafluoroethyllining lining stainless steel autoclave
Interior, system keeps 8h at 180 DEG C.The system for the treatment of is cooled to room temperature, and obtained dark brown liquid is centrifuged under 10000rpm
15min removes large granular impurity, and supernatant is taken to remove little particle impurity by the membrane filtration that aperture is 0.22 micron, obtains palm fibre
Color liquid is carbon dots solution.
Obtained carbon dots solution adds in pure water and is made into the carbon that concentration is 10mg/ml, 3mg/ml, 2mg/ml and 1mg/ml successively
Point sample, the carbon dots sample of various concentration have different double transmitting fluorescent characteristics.
As shown in Figure 1, fluorescence emission spectrum of the carbon dots sample of various concentration under 365nm excitation wavelengths.Fig. 1 (a) is
Concentration is the emission spectrum of 10mg/ml carbon dots solutions, shows that main emission peak is located at for F2 at 475nm, secondary peak is located at 440nm for F1
Place；Fig. 1 (b) is the emission spectrum that concentration is 3mg/ml carbon dots solutions, shows that two emission peaks F1 and F2 have identical intensity,
Wherein emission peak F1 is located at 435nm, and emission peak F2 is located at 470nm；Fig. 1 (c) is the hair that concentration is 3mg/ml carbon dots solutions
Spectrum is penetrated, shows that main emission peak is located at for F1 at 465nm, secondary peak is located at for F2 at 435nm；Fig. 1 (d) is that concentration is 1mg/ml carbon
The emission spectrum of point solution shows that main emission peak is located at for F1 at 430nm, and secondary peak is located at for F2 at 460nm.
With the reduction of concentration, the relative peak intensities of emission peak F1 and F2 are changed.When concentration is 10mg/ml,
F2 is main emission peak, and with the reduction of concentration, the transmitting peak intensity at F2 begins lower than the transmitting peak intensity at F1, when concentration reaches
To in 1mg/ml, carbon dots sample can be adjusted using F1 emission peaks as main emission peak by adjusting the concentration of carbon dots sample
Double transmitting fluorescent characteristics of sample are controlled, is conducive to carbon quantum dot and widely applies；On the other hand, emission peak F1 and F2 can be with
It the reduction of concentration and blue-shifted phenomenon occurs.
As shown in Fig. 2, the carbon dots sample of various concentration has apparent wide in range absworption peak at 315nm, carbon is illustrated
The n- π of point sample*Transition.
As shown in figure 3, infrared data shows to have on carbon dots surface very abundant surface group.In 1524cm and
Peak at 1642cm is respectively the stretching vibration of C=C and C=N keys, and the peak at 1460cm is CH2,1630cm and 1390cm
The peak at place is respectively belonging to C=O and C-O keys；Wide in range peak of the center at 3400cm is considered the stretching vibration of O-H and N-H, says
Bright to have abundant amino and hydroxyl on the surface of carbon dots, these groups ensure that the hydrophily of carbon dots.
As shown in figure 4, X-ray diffracting spectrum (XRD) shows sample, there are one apparent wide in range near 2 θ=20 ° angles
Peak, it is agraphitic carbon to illustrate carbon dots sample.
Embodiment 2：
It weighs 1g citric acids and 0.195g glycine (molar ratio 1: 0.5) is dissolved in the pure water of 10ml, magnetic agitation
10min is allowed to be formed uniformly transparent mixed solution, and mixed solution is transferred to polytetrafluoroethyllining lining stainless steel autoclave
Interior, system keeps 12h at 160 DEG C.The system for the treatment of is cooled to room temperature, and obtained dark brown liquid is centrifuged under 10000rpm
15min removes large granular impurity, and supernatant is taken to remove little particle impurity by the membrane filtration that aperture is 0.22 micron, obtains palm fibre
Color liquid is carbon dots solution.
Obtained carbon dots solution adds in pure water and is made into the carbon that concentration is 10mg/ml, 3mg/ml, 2mg/ml and 1mg/ml successively
Point sample, the carbon dots sample of various concentration have different double transmitting fluorescent characteristics.
Embodiment 3：
It weighs 1g citric acids and 0.098g glycine (molar ratio 1: 0.25) is dissolved in the pure water of 10ml, magnetic agitation
10min is allowed to be formed uniformly transparent mixed solution, and mixed solution is transferred to polytetrafluoroethyllining lining stainless steel autoclave
Interior, system keeps 12h at 180 DEG C.The system for the treatment of is cooled to room temperature, and obtained dark brown liquid is centrifuged under 10000rpm
15min removes large granular impurity, and supernatant is taken to remove little particle impurity by the membrane filtration that aperture is 0.22 micron, obtains palm fibre
Color liquid is carbon dots solution.
Obtained carbon dots solution adds in pure water and is made into the carbon that concentration is 10mg/ml, 3mg/ml, 2mg/ml and 1mg/ml successively
Point sample, the carbon dots sample of various concentration have different double transmitting fluorescent characteristics.
Claims (5)
1. a kind of double emission peak carbon quantum dots of concentration-dependant and preparation method, which is characterized in that be as follows：
(1) citric acid and glycine are dissolved in certain proportion in a certain amount of pure water, magnetic agitation 10min makes its mixing equal
It is even, form transparent mixed solution；
(2) transparent mixed solution in step (1) is taken to be transferred in the stainless steel autoclave of polytetrafluoroethyllining lining to carry out
Hydro-thermal reaction is cooled to room temperature after hydro-thermal reaction；
(3) product of step (2) is first removed into large granular impurity through centrifugation, then little particle impurity is removed through filter membrane, obtain brown
Filtrate, be carbon quantum dot solution；
(4) the carbon quantum dot solution obtained in step (3) addition pure water is made into the carbon quantum dot solution of various concentration.
2. a kind of double emission peak carbon quantum dots of concentration-dependant according to claim 1 and preparation method, which is characterized in that
The molar ratio of citric acid and glycine is 1: 0.25~1 in its step (1), and the volume of pure water used in dissolving is 10ml.
3. a kind of double emission peak carbon quantum dots of concentration-dependant according to claim 1 and preparation method, which is characterized in that
Hydrothermal temperature is 150 DEG C~180 DEG C in its step (2), and the reaction time is 3~12h.
4. a kind of double emission peak carbon quantum dots of concentration-dependant according to claim 1 and preparation method, which is characterized in that
Centrifugal rotational speed is 10000rpm, centrifugation time 15min in its step (3)；Filter membrane is the filter membrane in 0.22 micron of aperture.
5. a kind of double emission peak carbon quantum dots of concentration-dependant according to claim 1 and preparation method, which is characterized in that
The concentration of carbon quantum dot solution is followed successively by 10mg/ml, 3mg/ml, 2mg/ml, 1mg/ml in its step (4).
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110849859A (en) * | 2019-12-17 | 2020-02-28 | 山东农业大学 | Method for detecting dibutyl phthalate based on fluorescence ratio method of double-emission carbon quantum dot labeled aptamer |
| CN116099387A (en) * | 2023-02-28 | 2023-05-12 | 自然资源部第三海洋研究所 | Anti-pollution separation membrane and preparation method thereof |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103342347A (en) * | 2013-05-09 | 2013-10-09 | 江苏大学 | Preparation method of carbon quantum dots with high fluorescence property |
| CN106398691A (en) * | 2016-08-29 | 2017-02-15 | 北京化工大学 | pH-responsive double-peak emission carbon quantum dot nano-material and preparation method and application thereof |
-
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- 2017-12-28 CN CN201711499813.XA patent/CN108083258A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103342347A (en) * | 2013-05-09 | 2013-10-09 | 江苏大学 | Preparation method of carbon quantum dots with high fluorescence property |
| CN106398691A (en) * | 2016-08-29 | 2017-02-15 | 北京化工大学 | pH-responsive double-peak emission carbon quantum dot nano-material and preparation method and application thereof |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110849859A (en) * | 2019-12-17 | 2020-02-28 | 山东农业大学 | Method for detecting dibutyl phthalate based on fluorescence ratio method of double-emission carbon quantum dot labeled aptamer |
| CN110849859B (en) * | 2019-12-17 | 2021-03-23 | 山东农业大学 | Method for detecting dibutyl phthalate based on fluorescence ratio method of double-emission carbon quantum dot labeled aptamer |
| CN116099387A (en) * | 2023-02-28 | 2023-05-12 | 自然资源部第三海洋研究所 | Anti-pollution separation membrane and preparation method thereof |
| CN116099387B (en) * | 2023-02-28 | 2024-07-09 | 自然资源部第三海洋研究所 | Anti-pollution ultrafiltration membrane and preparation method thereof |
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Application publication date: 20180529 |