CN106566534B - A kind of feux rouges carbon dots and preparation method thereof with high yield and quantum yield - Google Patents
A kind of feux rouges carbon dots and preparation method thereof with high yield and quantum yield Download PDFInfo
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Abstract
The feux rouges carbon dots and preparation method thereof with high quality yield and quantum yield that the invention discloses a kind of, be one kind can largely synthesize red light region (peak value is between 610-661nm) it is inner transmitting and quantum yield be at present highest 76% carbon quantum dot preparation method.This kind of carbon nano-particles size is between 2-8nm, is mainly made of graphited carbon core and unbodied functional group's shell, and have good luminous efficiency, solubility and stability in common solvent.As a kind of novel red light flourescent material; it is low with production cost, can large-scale preparation, the excellent property such as luminous efficiency is high, stability is good, be most to be hopeful to can replace the hypotoxicity nanometer new material that traditional semiconductor-quantum-point plays a role in photoelectric device, fluorescence sense and biotechnology at present.
Description
Technical field
The invention belongs to technical field of nano material, and in particular to a kind of feux rouges carbon dots with high yield and quantum yield
And preparation method thereof.
Background technique
21 century is the epoch for being filled with opportunities and challenges, to the hair in the fields such as information, the energy, environment and national defence
Exhibition more stringent requirements are proposed, thus to Materials also proposed with day all into requirement.Wherein, the micromation of device, intelligence
Energyization requires that the size of material is smaller and smaller, therefore nano material rapidly becomes in new material research field to the future economy
It is the most active in the research object being had an important influence with social development, and contemporary basic research, closest to practical application
Field.Different from bulk material, nano material have many unique properties, as one of them photoluminescent property be even more by
Strong research interest.In recent years, the semiconductor-quantum-points such as relevant core-shell structure nanometer particle of CdSe, ZnS and CdSe because
Its unique optical property and extensive biomedical applications prospect have attracted everybody widely to pay close attention to.Semiconductor-quantum-point is in life
Fluorescence imaging on object repeatedly confirmed under lab, and clinically carries out the application of tumor marker and cutting all
There is successful precedent.However, this kind of quantum dot is all using heavy metal as indispensable element, especially Cd, even if extremely low dense
Degree is lower to be used, and huge harm can be also brought to natural environment and human health, to limit this kind of semiconductor-quantum-point
Application potential, development and application especially clinically.So finding a kind of completely new, with preferable optical property, less toxic
Property nano material come replace heavy metal semiconductor-quantum-point play a role just become it is necessary to.From carbon quantum dot in 2004
For the first time by since chancing on, it has just promptly attracted the strong interest of vast scientists.This is a kind of completely new, size
In 10 nanometers of carbon nanomaterials below, and have the advantageous property that semiconductor-quantum-point does not possess, mainly has: high
Blue-green fluorescent quantum yield, strong stability of photoluminescence, biologically inert and good bio-compatibility etc..Meanwhile carbon quantum
A large amount of functional group is contained on point surface, provides possibility for grafting other function molecule, has further expanded its application field,
To be considered to be the best replacer of other semiconductor-quantum-points.It is important to note that the main component of carbon quantum dot
For carbon, thus there is low-down toxicity, even if the toxicity still very little under the concentration of mg/ml rank.In addition, this kind of carbon
Nano material also has outstanding photoelectric conversion performance.These properties outstanding know that carbon quantum dot in biomarker, biology
Not, bio-imaging etc. has more broad application prospect.By the great efforts of scientists in recent years, about carbon amounts
Son point carbon source and synthetic method have been achieved for unprecedented development, the former mainly include glucose, ethyl alcohol, milk,
The organic substances such as coal;The method that the latter is related to mainly has hydro-thermal method, Microwave Digestion, laser ablation, calcination method and acid
Solution etc..Although thousands of carbon sources and preparation method up to a hundred are reported, carbon nano-particles prepared by the overwhelming majority are most
Good excitation and launch wavelength are all to be located at blue-green region, and absorption and hair in long wavelength region, especially red light region
Penetrate it is weaker, this prepare bottleneck not only in biomedical applications cell and biological tissue bring serious light injury,
And there are the critical defects such as tissue penetration and signal resolution be low, carbon quantum dot is seriously hindered in biomedicine
With the application development in the fields such as photoelectric device.Although although currently, have a few report carbon quantum dot have red fluorescence,
But its quantum yield is often below 10%, and launch wavelength is typically not greater than 620nm, more seriously, means of purification
It can be related to the technologies such as the very low column chromatography of separative efficiency and dialysis.Therefore, find it is a kind of simplicity, it is can amplifying, efficiently
, intense red fluorescent carbon quantum dot can be prepared method it is just very crucial.Synthetic method proposed by the present invention can be effective
Solve above-mentioned problem.
Summary of the invention
Goal of the invention: in order to overcome the deficiencies in the prior art, the present invention provides a kind of with high yield and quantum
Feux rouges carbon dots of yield and preparation method thereof, this nanoparticle by graphitized area and surface in core amorphous domain two
Part forms, their core diameter length is between 2-8 nanometers, and outer casing thickness is to be shown generally as more between 1-3 nanometers
The torispherical structure of layer graphene composition.
Technical solution: to achieve the above object, the technical solution adopted by the present invention are as follows:
A kind of feux rouges carbon dots with high yield and quantum yield are made of spherical the shell of internal core and its outside
Body, the core are graphited carbon, and the shell is amorphous functional group, and the kernel is with shell by being covalently keyed;
Wherein, the diameter of the core be 2~8nm, the shell with a thickness of 1~3nm.
Further, the carbon core is Multi-layer graphite structure, and average aromatic region area is 4nm.
Further, the amorphous functional group in the shell be hydrophilic functional group, including hydroxyl, amino, carboxyl and
Carbonyl.
Further, which has absorption and transmitting in visible light region, the red under the light source activation of 460-600nm
Fluorescent carbon point, Fluorescent peal is between 610-661nm.
The preparation method of the above-mentioned feux rouges carbon dots with high yield and quantum yield, comprises the following specific steps that:
(1) solvent-thermal method prepares red fluorescence carbon quantum dot mixture
Formamide 5-15ml is put into centrifuge tube, and citric acid 0.2-0.6g and ethylenediamine 100-1300 μ L is added, and concussion is dissolved,
Mixed liquor is transferred in the autoclave containing 80mL dimethyl sulfoxide, shakes up and is sealed;
Baking oven is preheated to 160-220 DEG C, and the autoclave is put into baking oven and reacts 4-24h, and end of reaction is turned off
Baking oven, cooled to room temperature;
(2) sedimentation separation red fluorescence carbon quantum dot
The mixed liquor obtained in step (1) is subjected to primary filtration, acetone 40-80mL is then added and shakes, is formed outstanding
Turbid;The black solid powder of red fluorescence carbon quantum dot is obtained again by centrifugal treating;It, will after acetone 5-10mL washing
It is scattered in dissolution solvent, is sealed.
Further, in step (2), the condition of the centrifugal treating is with 5000-10000 revs/min of revolving speed progress 5-
10 minutes.
Further, in step (2), the dissolution solvent is deionized water or dimethyl sulfoxide.
Further, in step (1), the optimum feed stock ratio of the citric acid and ethylenediamine is 0.4g:700 μ L.
It further, is 45-76% according to the obtained quantum yield of this method, carbon quantum dot mass yield after purification
For 29-84%.
The utility model has the advantages that a kind of feux rouges carbon dots and preparation method thereof with high yield and quantum yield provided by the invention,
Be one kind can largely synthesize red light region (peak value is between 610-661nm) it is inner transmitting and quantum yield be at present it is highest
The preparation method of 76% carbon quantum dot (abbreviation carbon dots).This kind of carbon nano-particles size is between 2-8nm, mainly by graphite
The carbon core of change and unbodied functional group's shell are formed, and have good luminous efficiency, solubility in common solvent
And stability.As a kind of novel red light flourescent material, have production cost it is low, can large-scale preparation, luminous efficiency pole
High, the excellent property such as stability is good is current to be most hopeful to can replace traditional semiconductor-quantum-point in photoelectric device, glimmering
The hypotoxicity nanometer new material to play a role in light sensing and biotechnology.
Detailed description of the invention
(a) is the transmission electron microscope photo of embodiment 1 in Fig. 1, and illustration is high-resolution-ration transmission electric-lens photo.It can from figure
To 3-4 nanometers of interior nuclear diameter average out to of carbon quantum dot, see that the spacing of lattice of carbon quantum dot is 0.21 nanometer in illustration, it is corresponding
In 100 lattice planes of graphite, the graphitization nuclear structure of carbon quantum dot is further confirmed.It (b) is that atomic force in embodiment 1 is aobvious
Micro- photo, the graphite flake that display carbon quantum dot height is 3-4 layers.
Fig. 2 is the solid state powder figure of the feux rouges carbon dots of embodiment 1 (quality of starting carbon source is 1.0g).It can from figure
It arrives, carbon quantum dot after purification is mainly black, is more importantly, by mass measurement, the mass yield of carbon dots can reach
To 80%, there are the potentiality for expanding preparation.
Fig. 3 is the UV absorption and fluorescence spectrum of the feux rouges carbon dots in embodiment 1.Carbon quantum dot exists as we can see from the figure
There is very strong absorption in visible light region, and obtained the maximum absorption is at 565nm;Simultaneously it can also be seen that the fluorescence peak of sample is
Independent of the transmitting of excitation, peak position is mainly at 654nm.
Fig. 4 is photo of the feux rouges carbon dots under natural light in embodiment 1.Carbon quantum dot is in visible light as we can see from the figure
The fact that can issue bright red fluorescence down, further demonstrate the high quantum yield of sample.
Specific embodiment
The present invention is specially that one kind can be synthesized largely and emit and measure red light region (peak value is between 610-661nm) be inner
The carbon quantum dot (abbreviation carbon dots) and preparation method thereof that sub- yield is at present highest 76%.This kind of carbon nano-particles size is in
Between 2-8nm, mainly it is made of graphited carbon core and unbodied functional group's shell, and have very in common solvent
Good luminous efficiency, solubility and stability.
The present invention is a kind of " graphite-amorphous carbon " hud typed red light Nano particle, and core is graphited carbon, diameter
It can be distributed in 2~8 nanometer ranges, shell is amorphous functional group, and thickness can be adjusted in 1~3 nanometer range, kernel
With shell by being covalently keyed.Wherein, carbon core is the Multi-layer graphite structure of highly crystalline, and aromatic region area is compared to it
He reports that carbon quantum dot is bigger than normal.In addition, the amorphous structure in shell contains the parents such as a large amount of hydroxyl, amino, carboxyl and carbonyl
Aqueous functional group.
Used solvent is dimethyl sulfoxide during the preparation of feux rouges carbon quantum dot of the invention, rather than other are logical
The water and ethyl alcohol equal solvent being often used.Dimethylsulfoxide solvent can prepare feux rouges carbon dots, and water and ethyl alcohol cannot, and select
Selecting it facilitates precipitation and separation sample.Preparation method specifically includes following specific steps:
(1) solvent-thermal method prepares red fluorescence carbon quantum dot mixture:
It first measures 5-15 milliliters of formamides to be put into 50 milliliters of centrifuge tube, then weighs a certain amount of citric acid respectively
(0.2-0.6 grams) and a certain amount of ethylenediamine (100-1300 μ L) are added in centrifuge tube, and concussion will be mixed up to being completely dissolved
Liquid is transferred in the autoclave containing 80mL dimethyl sulfoxide, is sealed;After high temperature oven is first preheated to certain temperature
(160-220 degrees Celsius), then reaction kettle is put into baking oven and reacts several hours (4-24 hours), end of reaction turns off baking oven,
Cooled to room temperature.
(2) sedimentation separation red fluorescence carbon quantum dot:
The mixed liquor obtained in step (1) is subjected to primary filtration, to remove not reacted impurity;Add 40-
The acetone of 80mL and concussion form suspension;Then, again by centrifugal treating (5000-10000 revs/min, 5-10 minutes)
Obtain the black solid powder of red fluorescence carbon quantum dot;After 2-4 5-10mL acetone washing of experience, distribute it to from
In the dissolution solvents such as sub- water and dimethyl sulfoxide, it is sealed.
According to above-mentioned preparation and separation method, we obtain a kind of red under the light source activation of 460-600nm
Fluorescent carbon point, for their Fluorescent peal between 610-661nm, quantum yield is up to 45-76%.It is calculated by quality versus
(using citric acid as substrate), carbon quantum dot mass yield after purification are up to 81%.This kind of carbon quantum dot has similar structure
Ingredient, average-size are about 4nm, are mainly shown as spherical shape on pattern.Meanwhile there is extremely strong optical stability, in biology
The fields such as medicine and photoelectric device have a wide range of applications.
Specific experiment effect, by the way that the present invention will be further explained below with reference to embodiment and attached drawing.
Embodiment 1
(1) mixed solution containing red fluorescence carbon dots is prepared
First 0.4g citric acid is put into the conical flask of 100mL, adds the formamide solvent of 10mL, is formed by oscillation
Transparent solution;Then, the ethylenediamine of 0.7mL is added, further vibrates, keeps sample dispersion uniform.Then, by transparent mixing
Liquid is transferred to the stainless steel cauldron (150 milliliters) containing 80mL dimethyl sulfoxide Nei, is sealed.First high temperature oven is preheated to
After 190 degrees Celsius (heating rate: 5 DEG C/min), then stainless steel cauldron is put into baking oven and reacts 6 hours, reacted
Finish, turn off baking oven, opens oven door, cooled to room temperature.
(2) mixed solution containing red fluorescence carbon dots is purified
The mixed liquor obtained after reaction in step (1) is first filtered processing, with remove unreacted impurity and
The bulky grain of formation.Then filtrate is transferred in the conical flask of 100mL, volume is about 25mL, is slow added into 40mL's
Acetone, solution system can gradually become cloudy at this time, and static 1 hour, it can be seen that a large amount of black precipitate is arranged at conical flask bottom,
Black precipitate is obtained again by centrifugal treating (5000 revs/min, 10 minutes).Finally, by the carbon quantum dot powder of acquisition
It is washed 3 times with the acetone soln of 2mL every time, more clean carbon quantum dot sample can be obtained.Sample both can be as solid
Powder storage can also be distributed in water and dimethyl sulfoxide isopolarity solvent, so as to later period use.The red fluorescence carbon obtained eventually
The launch wavelength of point is 654 nanometers, and quantum yield and mass yield are respectively as follows: 76% and 81%.
As shown in Figure 1,2,3, 4, in Fig. 1 (a) be embodiment 1 transmission electron microscope photo, illustration is high-resolution-ration transmission electric-lens
Photo.3-4 nanometers of interior nuclear diameter average out to of carbon quantum dot as we can see from the figure, see in illustration between the lattice of carbon quantum dot
Away from being 0.21 nanometer, corresponding to 100 lattice planes of graphite, the graphitization nuclear structure of carbon quantum dot is further confirmed.It (b) is real
Apply the atomic force micrograph in example 1, the graphite flake that display carbon quantum dot height is 3-4 layers.
Fig. 2 is the solid state powder figure of the feux rouges carbon dots of embodiment 1 (quality of starting carbon source is 1.2g).It can from figure
It arrives, carbon quantum dot after purification is mainly black, is more importantly, passes through mass measurement, the mass yield energy of carbon quantum dot
Enough reach 80%, there are the potentiality for expanding preparation.
Fig. 3 is the UV absorption and fluorescence spectrum of the feux rouges carbon dots in embodiment 1.Carbon quantum dot exists as we can see from the figure
There is very strong absorption in visible light region, and obtained the maximum absorption is at 565nm;Simultaneously it can also be seen that the fluorescence peak of sample is
Independent of the transmitting of excitation, peak position is mainly at 654nm.
Fig. 4 is photo of the feux rouges carbon dots under natural light in embodiment 1.Carbon quantum dot is in visible light as we can see from the figure
The fact that can issue bright red fluorescence down, further demonstrate the high quantum yield of sample.
Embodiment 2
Preparation method and embodiment 1 are identical, but reaction temperature is changed to 220 DEG C, and other conditions are constant, finally obtained red
The launch wavelength of color fluorescent carbon point is 661 nanometers.Launch wavelength compared to 190 DEG C, red shift 7 nanometers, this is attributed to higher
Reaction temperature caused by higher degree of graphitization.Meanwhile the quantum yield after integrating sphere measurement but drops to 45%, this
Outside, mass yield, that is, sample yield is also improved, and reaches 84%.From the results of view, raising reaction temperature can generate slight
Emit the increase of red shift and mass yield, and reduces quantum yield.
Embodiment 3
Preparation method and embodiment 1 are identical, but when reaction temperature is reduced to 160 DEG C, other conditions are constant, final
The launch wavelength of the red fluorescence carbon dots arrived is 631 nanometers, is 59% by the specific quantum yield that integrating sphere is calculated, passes through title
The mass yield for restoring sample is 43%.From the results of view, it reduces reaction temperature and produces blue shift and amount to launch wavelength
The decline result of sub- yield and sample yield.Therefore, in the preparation process of this nano material, control reaction temperature is very
Crucial, severely impact the Formation history and constituent of carbon quantum dot.
Embodiment 4
Preparation method and embodiment 1 are identical, but the ratio of feed change ratio, i.e. citric acid and ethylenediamine is 0.4g:
0.1mL.Obtaining launch wavelength under this condition is 610 nanometers, corresponding quantum yield and sample quality yield are as follows: 18% He
29%.It can be seen that it is unfavorable that the above three index of carbon quantum dot has the tendency that when ethylenediamine volume is inadequate, illustrate raw material
Ratio be also to prepare the key of high performance carbon quantum dot.Therefore material rate is carefully studied to the property shadow of such nano material
It is also necessary for ringing.
Embodiment 5
Preparation method and embodiment 1 are identical, but the ratio of feed change ratio, i.e. citric acid and ethylenediamine is 0.4g:
0.3mL.Obtaining launch wavelength at this time is 627 nanometers, corresponding quantum yield and sample quality yield are as follows: 48%53%.Thus
As it can be seen that the photoluminescent property and mass yield of prepared carbon nanomaterial have when the ratio shared by the raw material ethylenediamine rises
The trend of raising.It is presumed that being because more ethylenediamines take part in the formation of carbon quantum dot.
Embodiment 6
Preparation method and embodiment 1 are identical, but the ratio of feed change ratio, i.e. citric acid and ethylenediamine is 0.4g:
0.5mL.Obtaining launch wavelength at this time is 639 nanometers, corresponding quantum yield and sample quality yield are as follows: 54% and 65%.By
This is as it can be seen that the photoluminescent property and quality of prepared carbon nanomaterial produce when the ratio shared by the raw material ethylenediamine continues to rise
Rate has the tendency that continuing to improve.
Embodiment 7
Preparation method and embodiment 1 are identical, but the ratio of feed change ratio, i.e. citric acid and ethylenediamine is 0.4g:
0.7mL.Obtaining launch wavelength at this time is 654 nanometers, corresponding quantum yield and sample quality yield are as follows: 76% and 81%.By
This is as it can be seen that the photoluminescent property and quality of prepared carbon nanomaterial produce when the ratio situation thus shared by the raw material ethylenediamine
Rate has all reached fabulous level.
Embodiment 8
Preparation method and embodiment 1 are identical, but the ratio of feed change ratio, i.e. citric acid and ethylenediamine is 0.4g:
0.9mL.Obtaining launch wavelength at this time is 656 nanometers, corresponding quantum yield and sample quality yield are as follows: 63% and 65%.By
This is as it can be seen that when the ratio shared by the raw material ethylenediamine is more than optimum value, the quantum yield and quality of prepared carbon nanomaterial
The slight decline of yield, and launch wavelength does not move substantially.
Embodiment 9
Preparation method and embodiment 1 are identical, but the ratio of feed change ratio, i.e. citric acid and ethylenediamine is 0.4g:
1.1mL.Obtaining launch wavelength at this time is 658 nanometers, corresponding quantum yield and sample quality yield are as follows: 59% and 57%.By
This as it can be seen that when the ratio shared by the raw material ethylenediamine continues to be more than optimum value, the launch wavelength of prepared carbon nanomaterial and
Quantum yield substantially remains unchanged, and mass yield continues to decline, and may be attributed to when washing excessive ethylenediamine
Also a part of sample is had lost.
Embodiment 10
Preparation method and embodiment 1 are identical, but the ratio of feed change ratio, i.e. citric acid and ethylenediamine is 0.4g:
1.3mL.Obtaining launch wavelength at this time is 658 nanometers, corresponding quantum yield and sample quality yield are as follows: 47% and 53%.By
This as it can be seen that when the ratio shared by the raw material ethylenediamine continues to be more than optimum value, the launch wavelength of prepared carbon nanomaterial and
Quantum yield substantially remains unchanged, and mass yield continues to decline, and may be attributed to when washing excessive ethylenediamine
Also a part of sample is had lost.
Above-described embodiment can be summarized as a table:
1 embodiment data statistic of table
The present invention uses solvent-thermal method (reaction kettle), synthesis side during preparing intense red fluorescent carbon point
Method is simple, environmentally protective, and the raw material used are cheap, and reaction temperature is between 160-220 DEG C, in addition, purifying is used
Organic sedimentation not only rapidly and efficiently but also yield is high, therefore such preparation method has very big industrial production prospect.
Meanwhile the carbon source used during reaction is not only from a wealth of sources, but also is entirely Green Chemistry.During purification
It only needs to carry out at normal temperature, it is only necessary to use relatively inexpensive organic reagent (acetone), and the amount used is also smaller, simultaneously
These reagents can be reused further after simply distilling, thus the very big cost reduced in production process.
Red fluorescence carbon dots prepared by the present invention do not have any difference compared with other carbon dots reported on composition, main
If carbon nucleus area obviously becomes larger.These carbon dots contain a large amount of hydrophilic functional group, thus can water, ethyl alcohol,
There is good solubility in formamide, N,N-dimethylformamide isopolarity solvent.Meanwhile in wider pH value (2-12) model
Under the conditions of enclosing interior, higher ionic strength, the irradiation of the high intensity ultraviolet of long period and long-time storage etc., carbon dots are red
The intensity of fluorescence and peak position will not substantially change, these test results all prove its biomedicine, photoelectric device,
Application with the fields such as visible light catalytic above has very extensive prospect.
The a length of 566nm of red fluorescence carbon dots optimum excitation wave prepared by the present invention, best launch wavelength is in 654nm.It is most
Good excitation and transmitting are all in visible light region, brought biological damage when efficiently avoiding using traditional ultraviolet light.
In addition, carbon dots quantum yield with higher, the quantum yield with higher in formamide, value can reach 76%,
Be report at present it is highest.In water phase, quantum yield can also be up to 43%.These carbon quantum dots are shown independent of sharp
The transmitting of hair, the position of fluorescence peak are not moved substantially.Follow-up study proves the red fluorescence of carbon dots mainly from graphite
The synergistic effect of the surface state of carbon core and the surface functional group composition of change.
Red fluorescence carbon dots prepared by the present invention have low-down toxicity, dense to the semilethal of human cervical cancer cell
Degree is 3-4 mg/ml, low 3 numbers out than the corresponding toxicities for the semiconductor-quantum-point (CdSe and CdTe) largely reported
It is more than magnitude.Therefore, the carbon dots of such method preparation are in the case where biomedicine needs concentration, completely will not influence cell growth and
Form, or even sometimes become the nutritious carbon sourc of cell.
The above is only a preferred embodiment of the present invention, it should be pointed out that: for the ordinary skill people of the art
For member, various improvements and modifications may be made without departing from the principle of the present invention, these improvements and modifications are also answered
It is considered as protection scope of the present invention.
Claims (5)
1. a kind of preparation method of the feux rouges carbon dots with high yield and quantum yield, it is characterised in that: including following specific step
It is rapid:
(1) solvent-thermal method prepares red fluorescence carbon quantum dot mixture
Formamide 5-15ml is put into centrifuge tube, and citric acid 0.2-0.6g and ethylenediamine 100-1300 μ L is added, and concussion dissolution will mix
It closes liquid to be transferred in the autoclave containing 80mL dimethyl sulfoxide, shakes up and be sealed;
Baking oven is preheated to 160-220 DEG C, and the autoclave is put into baking oven and reacts 4-24h, and end of reaction turns off baking
Case, cooled to room temperature;
(2) sedimentation separation red fluorescence carbon quantum dot
The mixed liquor obtained in step (1) is subjected to primary filtration, acetone 40-80mL is then added and shakes, forms suspension;
The black solid powder of red fluorescence carbon quantum dot is obtained again by centrifugal treating;After acetone 5-10mL washing, by its point
It dissipates in dissolution solvent, is sealed;
It is 45-76% according to the obtained quantum yield of this method, carbon quantum dot mass yield after purification is 29-84%.
2. the preparation method of the feux rouges carbon dots according to claim 1 with high quality yield and quantum yield, feature
Be: in step (2), the condition of the centrifugal treating be with 5000-10000 revs/min of revolving speed progress 5-10 minutes.
3. the preparation method of the feux rouges carbon dots according to claim 1 with high yield and quantum yield, it is characterised in that:
In step (2), the dissolution solvent is deionized water or dimethyl sulfoxide.
4. the preparation method of the feux rouges carbon dots according to claim 1 with high yield and quantum yield, it is characterised in that:
In step (1), the optimum feed stock ratio of the citric acid and ethylenediamine is 0.4g: 700 μ L.
5. the preparation method of the feux rouges carbon dots according to claim 1 to 4 with high yield and quantum yield is prepared into
Feux rouges carbon dots, it is characterised in that: by internal core and its orbicule that forms of shell of outside, the core is graphited
Carbon, the shell are amorphous functional group, and the kernel is with shell by being covalently keyed;Wherein, the diameter of the core is 2
~8nm, the shell with a thickness of 1~3nm;
The carbon core is Multi-layer graphite structure, and average aromatic region area is 4 nm;
Amorphous functional group in the shell is hydrophilic functional group, is any one of hydroxyl, amino, carboxyl and carbonyl;
The carbon dots have absorption and transmitting in visible light region, the red fluorescence carbon dots under the light source activation of 460-600nm, fluorescence
Peak is between 610-661nm.
Priority Applications (2)
Application Number | Priority Date | Filing Date | Title |
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CN201610965433.XA CN106566534B (en) | 2016-11-04 | 2016-11-04 | A kind of feux rouges carbon dots and preparation method thereof with high yield and quantum yield |
PCT/CN2017/000665 WO2018082204A1 (en) | 2016-11-04 | 2017-11-03 | Red-emitting carbon dot having high yield and quantum yield and preparation method therefor |
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