CN108384538A - A kind of preparation method of fluorescent carbon quantum dot - Google Patents
A kind of preparation method of fluorescent carbon quantum dot Download PDFInfo
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- CN108384538A CN108384538A CN201810102306.6A CN201810102306A CN108384538A CN 108384538 A CN108384538 A CN 108384538A CN 201810102306 A CN201810102306 A CN 201810102306A CN 108384538 A CN108384538 A CN 108384538A
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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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- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
Abstract
The present invention provides a kind of preparation methods of fluorescent carbon quantum dot, include the following steps：A, using sorbose as carbon source, sorbose is added in the mixed solution of second alcohol and water, and be sufficiently mixed uniformly；Wherein, sorbose: the volume ratio of mixed solution=0.5 of second alcohol and water ~ 4g: 50mL, second alcohol and water are 1: 1 ~ 3；B, the mixed liquor obtained by step a is placed in reaction kettle, 2 ~ 8h of hydro-thermal reaction is cooled to room temperature after reaction under the conditions of 170 ~ 200 DEG C, obtains reaction solution；C, reaction solution is placed in 1 ~ 3d of dialysis in bag filter after filtering, obtain the aqueous solution of target carbon quantum dot；D, target carbon quantum dot is obtained after being dried in vacuo the aqueous solution of above-mentioned carbon quantum dot.The present invention has the advantages such as synthesis technology is simple, condition is easily controllable, obtained carbon quantum dot fluorescent stability is good, and emission wavelength adjustable extent is wider using sorbose as carbon source.
Description
Technical field
The present invention relates to nanometer material science fields, relate in particular to a kind of preparation method of fluorescent carbon quantum dot.
Background technology
Carbon quantum dot (CQD) is a kind of size in 10nm or less and the fluorescent carbon granule crystal of monodispersity, is to have amount
Sub- dimensional effect, small-size effect, the nano size particles of skin effect.As a kind of novel semiconductor nano material, with
Traditional inorganic semiconductor quantum dot is compared, and has photochemical stability strong, and emission wavelength range is adjustable, and biocompatibility is strong,
And the advantages such as cytotoxicity is low, it has a wide range of applications on Element detection, biomarker, bio-sensing, luminescent device.
Currently, there are many preparation method for the carbon quantum dot that people have worked out, according to the difference of carbon source, mainly have following
Two kinds：
One is the preparation method with glucose, fructose etc. for carbon source, this method usually requires that complicated organic examination is added
Agent or precious metal ion, not only preparation process is complicated, is difficult to control, of high cost, and organic reagent and easy pair of precious metal ion
Carbon dots pollute, and cause impurity more.
Another kind is the preparation method using organic waste materials as carbon source, such as：Application No. is 201210264411.2 patents
File discloses a kind of preparation method of luminescence generated by light carbon quantum dot, and using bean dregs powder as carbon source, bean dregs powder is placed in height
It presses in kettle, the carbonization of 200 DEG C of progress 20min~40min in drying box, obtained crude product is ground, molecular sieve selects,
Centrifugation, dissolving, finally obtain luminescence generated by light carbon quantum dot aqueous solution；Application No. is 201510147558.7 patent documents to disclose
A kind of using corncob as the method for carbon source one-step synthesis fluorescent carbon point, preparation process needs that ethylenediamine reagent is added；Application
Number patent document for being 201610836757.3 discloses a kind of using cane molasses as the preparation side of Material synthesis fluorescent carbon point
Method and application.Above-mentioned preparation method has in common that its carbon source is the substance of more phenyl ring, phenyl ring oleophyllie hydrophobic, this knot
Structure is unfavorable for the separating-purifying of carbon dots, and seriously affects the research to carbon dots optical characteristics, is especially extremely disadvantageous to test
's.
Carbon quantum dot prepared by existing preparation method with its excellent biocompatibility, nontoxic, emission wavelength range is adjustable
And it is easy to the speciality such as surface-functionalized, in multiple fields instead of the application of conventional semiconductors quantum dot, still, still have
Emission wavelength adjustable extent is relatively narrow, the relatively narrow problem of especially available wave-length coverage.
Invention content
It is an object of the invention to provide a kind of preparation methods of fluorescent carbon quantum dot, to solve existing method preparation process
Complexity, the relatively narrow problem of gained fluorescent carbon quantum dot emission wavelength adjustable extent.
The purpose of the present invention is what is be achieved through the following technical solutions：A kind of preparation method of fluorescent carbon quantum dot, including
Following steps：
A, using sorbose as carbon source, sorbose is added in the mixed solution of second alcohol and water, and be sufficiently mixed uniformly；Its
In, sorbose: the volume ratio of mixed solution=0.5 of second alcohol and water~4g: 50mL, second alcohol and water are 1: 1~3；
B, the mixed liquor obtained by step a is placed in reaction kettle, 2~8h of hydro-thermal reaction under the conditions of 170~200 DEG C, instead
It after answering, is cooled to room temperature, obtains reaction solution；
C, reaction solution is placed in 1~3d of dialysis in bag filter after filtering, obtain the aqueous solution of target carbon quantum dot；
D, target carbon quantum dot is obtained after being dried in vacuo the aqueous solution of above-mentioned carbon quantum dot.
In step a of the present invention, the ethyl alcohol is the absolute ethyl alcohol of chromatographic grade, and water is ultra-pure water.
In step a of the present invention, after sorbose to be added to the mixed solution of second alcohol and water, first heating stirring makes sorbose
Dissolving, then 15~20min of ultrasonic mixing again.
In step b of the present invention, the temperature of hydro-thermal reaction is 180 DEG C, reaction time 4h.
In step c of the present invention, the filter membrane is the teflon membrane filter of aperture 0.22um.
In step c of the present invention, the specification of the bag filter is WM1000.
The present invention has the following advantages：
1, for the present invention using sorbose as carbon source, the hydroxyl decomposed using sorbose itself has carried out surface modification to carbon dots,
And water-soluble carbon dots are obtained by one step of hydro-thermal method, with raw material is cheap, synthesis technology is simple, condition is easily controllable, economic ring
The advantages such as guarantor, avoid the pollution that the modification of organic matter etc. in the prior art is brought, reduce the influence of impurity.
2, the separating-purifying process of carbon quantum dot of the present invention is relatively simple, avoids centrifugation cumbersome in the prior art, layer
The means such as analysis, since all carbon quantum dots are nucleated and grow up under the conditions of identical pressure and temperature, granularity is very
Uniformly.
3, the present invention is good as carbon quantum dot fluorescent stability made from carbon source using sorbose, and yield and luminous efficiency are high, point
It dissipates that property is good, the ratio and excitation wavelength for adjusting second alcohol and water can be passed through so that the wavelength of transmitted light of carbon quantum dot is from blue light
Gradually change to yellow light, emission wavelength adjustable extent is wider, and with the variation of excitation spectrum, the luminous intensity variations of sample compared with
It is small, application value higher.
Description of the drawings
Fig. 1 is the transmission electron microscope picture of 1 gained carbon quantum dot of embodiment.
Fig. 2 is the Fourier infrared absorption spectrum of 1 gained carbon quantum dot of embodiment.
Fig. 3 is launching light spectrogram of the 1 gained carbon quantum dot of embodiment under different exciting lights.
Fig. 4 is launching light spectrogram of the 1 gained carbon quantum dot of comparative example under different exciting lights.
Specific implementation mode
The preparation method of fluorescent carbon quantum dot of the present invention is described in detail with specific embodiment below.
Embodiment 1：
(1) the chromatographic grade absolute ethyl alcohol 25mL that purity is 99.8% is mixed with ultra-pure water 25mL and is placed in 100mL beakers,
2g sorboses are added, heating stirring makes sorbose dissolve.Then further ultrasonic mixing 20min after beaker mouth being sealed.
(2) mixed solution after ultrasound is placed in the brown polytetrafluoroethyllining lining of 100mL, is sealed in corresponding high pressure
In reaction kettle, the heating progress hydro-thermal reaction in high temperature drying case, reaction temperature is 180 DEG C, time 4h.
(3) reaction solution after pyrolysis being carbonized is filtered by the polytetrafluoroethylene (PTFE) filter tip of 0.22um, is subsequently placed in WM1000
Bag filter in, and dialyse 2d in ultra-pure water to get to the aqueous solution of carbon quantum dot.
(4) target carbon quantum dot is obtained after being dried in vacuo the aqueous solution of above-mentioned carbon quantum dot.
The characterization of correlated performance is carried out to above-mentioned carbon quantum dot, as a result as shown in FIG. 1 to 3, wherein Fig. 1 shows carbon amounts
Son point granularity is highly uniform, and Fig. 2 shows that the groups such as hydroxyl are contained on carbon quantum dot surface.The part luminescent properties data of carbon quantum dot
And yield is as shown in table 1, wherein yield indicates the percentage of the quality and carbon source quality used of final carbon quantum dot.
Embodiment 2：
(1) the chromatographic grade absolute ethyl alcohol 17mL that purity is 99.8% is mixed with ultra-pure water 33mL and is placed in 100mL beakers,
2g sorboses are added, heating stirring makes sorbose dissolve.Then further ultrasonic mixing 20min after beaker mouth being sealed.
(2) mixed solution after ultrasound is placed in the brown polytetrafluoroethyllining lining of 100mL, is sealed in corresponding high pressure
In reaction kettle, the heating progress hydro-thermal reaction in high temperature drying case, reaction temperature is 180 DEG C, time 4h.
(3) reaction solution after pyrolysis being carbonized is filtered by the polytetrafluoroethylene (PTFE) filter tip of 0.22um, is subsequently placed in WM1000
Bag filter in, and dialyse 2d in ultra-pure water to get to the aqueous solution of carbon quantum dot.
(4) target carbon quantum dot is obtained after being dried in vacuo the aqueous solution of above-mentioned carbon quantum dot.
Correlated performance measurement is carried out to gained carbon quantum dot, and by the results are shown in Table 1.
Embodiment 3：
(1) chromatographic grade absolute ethyl alcohol 12.5mL and ultra-pure water 37.5mL that purity is 99.8% are mixed and is placed in 100mL burnings
In cup, 2g sorboses are added, heating stirring makes sorbose dissolve.Then further ultrasonic mixing 20min after beaker mouth being sealed.
(2) mixed solution after ultrasound is placed in the brown polytetrafluoroethyllining lining of 100mL, is sealed in corresponding high pressure
In reaction kettle, the heating progress hydro-thermal reaction in high temperature drying case, reaction temperature is 180 DEG C, time 4h.
(3) reaction solution after pyrolysis being carbonized is filtered by the polytetrafluoroethylene (PTFE) filter tip of 0.22um, is subsequently placed in WM1000
Bag filter in, and dialyse 2d in ultra-pure water to get to the aqueous solution of carbon quantum dot.
(4) target carbon quantum dot is obtained after being dried in vacuo the aqueous solution of above-mentioned carbon quantum dot.
Correlated performance measurement is carried out to gained carbon quantum dot, and by the results are shown in Table 1.
Comparative example 1：
(1) the chromatographic grade absolute ethyl alcohol 25mL that purity is 99.8% is mixed with ultra-pure water 25mL and is placed in 100mL beakers,
2g glucose is added, heating stirring makes glucose dissolve.Then further ultrasonic mixing 20min after beaker mouth being sealed.
(2) mixed solution after ultrasound is placed in the brown polytetrafluoroethyllining lining of 100mL, is sealed in corresponding high pressure
In reaction kettle, the heating progress hydro-thermal reaction in high temperature drying case, reaction temperature is 180 DEG C, time 4h.
(3) reaction solution after pyrolysis being carbonized is filtered by the polytetrafluoroethylene (PTFE) filter tip of 0.22um, is subsequently placed in WM1000
Bag filter in, and dialyse 2d in ultra-pure water to get to the aqueous solution of carbon quantum dot.
(4) target carbon quantum dot is obtained after being dried in vacuo the aqueous solution of above-mentioned carbon quantum dot.
Correlated performance measurement is carried out to gained carbon quantum dot, and by the results are shown in Table 1.
Table 1：
Claims (6)
1. a kind of preparation method of fluorescent carbon quantum dot, characterized in that include the following steps：
A, using sorbose as carbon source, sorbose is added in the mixed solution of second alcohol and water, and be sufficiently mixed uniformly；Wherein,
Sorbose: the volume ratio of mixed solution=0.5 of second alcohol and water ~ 4g: 50mL, second alcohol and water are 1: 1 ~ 3；
B, the mixed liquor obtained by step a is placed in reaction kettle, 2 ~ 8h of hydro-thermal reaction under the conditions of 170 ~ 200 DEG C, reaction terminates
Afterwards, it is cooled to room temperature, obtains reaction solution；
C, reaction solution is placed in 1 ~ 3d of dialysis in bag filter after filtering, obtain the aqueous solution of target carbon quantum dot；
D, target carbon quantum dot is obtained after being dried in vacuo the aqueous solution of above-mentioned carbon quantum dot.
2. the preparation method of fluorescent carbon quantum dot according to claim 1, characterized in that in step a, the ethyl alcohol is color
The absolute ethyl alcohol of spectrum level, water are ultra-pure water.
3. the preparation method of fluorescent carbon quantum dot according to claim 1, characterized in that in step a, sorbose is added
To after the mixed solution of second alcohol and water, first heating stirring makes sorbose dissolve, then 15 ~ 20min of ultrasonic mixing again.
4. the preparation method of fluorescent carbon quantum dot according to claim 1, characterized in that in step b, the temperature of hydro-thermal reaction
Degree is 180 DEG C, reaction time 4h.
5. the preparation method of fluorescent carbon quantum dot according to claim 1, characterized in that in step c, the filter membrane is hole
The teflon membrane filter of diameter 0.22um.
6. the preparation method of fluorescent carbon quantum dot according to claim 1, characterized in that in step c, the bag filter
Specification is WM1000.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110155984A (en) * | 2019-06-12 | 2019-08-23 | 浙江科技学院 | Using soybean slag as the method and application of raw material hydro-thermal method synthesising biological matter fluorescent carbon point |
| CN111187618A (en) * | 2020-01-13 | 2020-05-22 | 山西大学 | Orange fluorescent carbon quantum dot and preparation method and application thereof |
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| CN110155984B (en) * | 2019-06-12 | 2021-02-02 | 浙江科技学院 | Method for synthesizing biomass fluorescent carbon dots by hydrothermal method with soybean dregs as raw material and application |
| CN111187618A (en) * | 2020-01-13 | 2020-05-22 | 山西大学 | Orange fluorescent carbon quantum dot and preparation method and application thereof |
| CN111187618B (en) * | 2020-01-13 | 2023-04-18 | 山西大学 | Orange fluorescent carbon quantum dot and preparation method and application thereof |
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