CN108085711A - A kind of preparation method of the carbon quantum dot to glow - Google Patents
A kind of preparation method of the carbon quantum dot to glow Download PDFInfo
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- CN108085711A CN108085711A CN201711390350.3A CN201711390350A CN108085711A CN 108085711 A CN108085711 A CN 108085711A CN 201711390350 A CN201711390350 A CN 201711390350A CN 108085711 A CN108085711 A CN 108085711A
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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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Abstract
The present invention relates to a kind of preparation methods of the carbon quantum dot to glow, comprise the following steps：1) solid base rear addition carbon source to be dissolved is added in organic solvent；2) by metal electrode inserting step 1) in acquired solution, with direct current or Alternating current discharges, reaction 15min 6h in whipping process；3) reaction solution is subjected to separation and purification treatment, obtains carbon quantum dot solution.The present invention is located at blue light or green wavelength mostly for the fluorescence of carbon quantum dot transmitting prepared by the prior art, the technical issues of luminescent color is single, preparation process of the invention have the advantages that low toxicity, good biocompatibility, at low cost, simple and environmentally protective.
Description
Technical field
The invention belongs to nanometer material science fields, and in particular to a kind of preparation method of the carbon quantum dot to glow.
Background technology
At present, carbon quantum dot due to its toxicity it is low, at low cost, good biocompatibility, cell imaging ability is strong, and raw material are rich
The advantages that rich, is concerned, and is widely used in bio-imaging, light emitting diode, color monitor and field of optoelectronic devices.
Report prepare fluorescent carbon quantum dot method it is very much, be broadly divided into method from top to bottom and from bottom to top method.From upper
And laxative remedy is exactly that big carbon skeleton structure is become small carbon skeleton structure by physico-chemical process；Method is that will have from bottom to top
Machine object forms carbon quantum dot particle by being dehydrated carbonization.But the fluorescence for the carbon quantum dot transmitting that these methods obtain at present is more
Positioned at blue light or green wavelength, (Kai Jiang, Shan Sun, Ling Zhang, Yue Lu, Aiguo Wu, Congzhong
Cai,and Hengwei Lin*.Red,Green,and Blue Luminescence by Carbon Dots:Full-
Color Emission Tuning and Multicolor Cellular Imaging Angew[J]
.Chem.Int.Ed.2015,54,1-5, this piece prepares carbon quantum dot using phenylenediamine)；And preparation process is complex, (Hai
Ming,Zheng Ma,Yang Liu,*Keming Pan,Hang Yu,Fang Wang and Zhenhui Kang*Large
scale electrochemical synthesis of high quality carbon nanodots and their
photocatalytic property Dalton Trans[J].The Royal Society of Chemistry 2012,
41,9526-9531, this prepares carbon quantum dot using maize leaves).Therefore, low toxicity, good biocompatibility, cost are sought
It is low, preparation is simple and environmentally protective new method prepares feux rouges carbon quantum dot and promotes carbon quantum dot in every respect
Using.
The content of the invention
The fluorescence emitted for carbon quantum dot prepared by the prior art is located at blue light or green wavelength, luminescent color mostly
The technical issues of single, the present invention provide one kind and glow carbon quantum dot preparation method, and preparation process of the invention has toxicity
Low, good biocompatibility, it is at low cost, simple and environmentally protective the advantages of.
The technical solution of the present invention：
A kind of preparation method of the carbon quantum dot to glow, is characterized in that and comprises the following steps：
1) solid base rear addition carbon source to be dissolved is added in organic solvent；
2) by metal electrode inserting step 1) in acquired solution, with direct current or Alternating current discharges in whipping process,
React 15min-6h；
3) reaction solution is subjected to separation and purification treatment, obtains carbon quantum dot solution.
Further, the carbon source in step 1) is benzene ring substance or alcohols.
Further, the metal electrode is platinum electrode.
Further, the organic solvent is methanol or ethyl alcohol.
Further, the solid base is sodium hydroxide or potassium hydroxide.
Further, the solid base and the mass ratio of carbon source are (0.1-0.7)：1.
Further, alternating current discharge voltage is 2200V-2640V, DC disruptive voltage 40V-60V.
Further, further include step 4) and feux rouges carbon quantum dot solution is subjected to rotary evaporation acquisition feux rouges carbon quantum solid point
Body powder.
Further, step 3) isolates and purifies specially：The precipitation of reaction solution bottom is removed, gained supernatant is
Feux rouges carbon quantum dot solution.
Further, the carbon source is indoles.
The present invention has advantageous effect：
1st, raw material benzene ring substance of the invention derives from a wealth of sources；
2nd, the fluorescent carbon quantum dot prepared by the present invention is under different excitation wavelengths, and launch wavelength is not with excitation wavelength
Change and change；
3rd, the optimal launch wavelength of fluorescent carbon quantum dot prepared by the present invention is 435nm, 460nm, 620nm and 610nm,
Double launch wavelengths are presented in middle benzene ring substance；
4th, the present invention prepares that feux rouges carbon quantum dot is nontoxic, at low cost, the cycle is short, preparation process is simple, environmentally protective；
5th, the present invention is a kind of new method for preparing feux rouges carbon quantum dot, contributes to the development in near-infrared fluorescent application.
Feux rouges carbon quantum dot is prepared using carbons substance and benzene ring substance, preparation method is simple, it is added in alcohol solution
Alkali process is discharged using platinum electrode, one-step synthesis.
6th, feux rouges carbon quantum dot electrochemically one-step synthesis, launches bright red under single excitation wavelength,
The method of this high yield has the advantages that low toxicity, good biocompatibility, at low cost, preparation process is simple, is widely used
Improving the field of biosensor, medical imaging devices and small light emitting diode.
Description of the drawings
Fig. 1 is the fluorescence spectra of the carbon quantum dot of the preparation of embodiment 1；
Fig. 2 is carbon quantum dot photo under light illumination prepared by embodiment 1；
Fig. 3 is the fluorescence spectra of carbon quantum dot prepared by embodiment 2；
Fig. 4 is the uv-visible absorption spectroscopy figure of carbon quantum dot prepared by embodiment 2；
Fig. 5 is the transmission electron microscope picture of carbon quantum dot prepared by embodiment 2；
Fig. 6 is the fluorescence spectra of control group 1；
Fig. 7 is the fluorescence spectra of control group 2；
Fig. 8 is the fluorescence spectra of control group 3；
Fig. 9 is the fluorescence spectra of carbon quantum dot prepared by embodiment 5；
Figure 10 is the fluorescence spectra of carbon quantum dot prepared by embodiment 6；
Figure 11 is the transmission electron microscope picture of carbon quantum dot prepared by embodiment 6.
Specific embodiment
Technical solution of the present invention is not limited to the specific embodiment of act set forth below, further include each specific embodiment it
Between any combination.Every equivalence changes done according to the technology of the present invention content and retouching, should be included in the skill of the present invention
Within art scope.
Embodiment 1：Indoles is chosen, is put into beaker, it is rear to add in absolute methanol and appropriate solid base；Then platinum electrode is inserted into
In solution, with direct current or Alternating current discharges in whipping process.After electric discharge, bottom precipitation is removed, then is the feux rouges of preparation
Carbon quantum dot solution.Indoles, absolute methanol and the solid base added in the present embodiment be not by any weighing (≤bases
Solubility in alcohols), principle is dissolved as with solid base.It is right using Fluorescence Spectrometer (LS 55, Perkin Elmer, USA)
Prepared feux rouges carbon quantum dot carries out Fluorescent Characterization, as shown in Figure 1.From Fig. 1 can red quantum dot solution obtained be in
Existing double transmitting launch wavelengths, under 360nm excitations, maximum emission peak is located at 415nm, under 580nm excitations, maximum emission peak
At 610nm.
Fig. 2 is the photo of the carbon quantum dot of the preparation of embodiment 1 under light illumination, and wherein left figure is that red carbon quantum dot solution exists
Picture under natural lamp, right figure is photo of the red carbon quantum dot solution under 532nm green lights, from Fig. 2 this it appears that institute
The carbon quantum dot solution of preparation can glow.
Embodiment 2：Indoles is selected as carbon source, weighs 1.32g indoles, 0.45g sodium hydroxides, 50mL absolute ethyl alcohols, insertion
Platinum electrode with Alternating current discharges 3.5h (voltage 2200V), takes upper solution, obtains feux rouges carbon quantum dot solution；Using fluorescence light
Spectrometer (LS 55, Perkin Elmer, USA) carries out Fluorescent Characterization to prepared feux rouges carbon quantum dot.As shown in figure 3, with not
This solution is excited with excitation wavelength, launch wavelength does not change with excitation wavelength and changed.Optimal excitation peak be located at 380nm and
At 580nm, corresponding optimal launch wavelength 435nm and 610nm.Uv-visible absorption spectroscopy TU-1901 (Beijing
Currency Instrumental Co.Ltd.Beijing, China) ultraviolet-visible spectrophotometer test, such as a left side of Fig. 4
Shown in figure and right figure, carbon quantum dot prepared by indoles all shows significantly to absorb in 200-600nm regions, in 218nm,
275nm, 288nm, 525nm, 573nm characteristic absorption peak are apparent.Transmission electron microscope picture (TEM-FEI, Tecnai G2, USA) such as Fig. 5
Shown, size is mainly distributed on 3-5nm.
Control group 1：
Indoles, sodium hydroxide and absolute ethyl alcohol blank：Indoles 1.32g, sodium hydroxide 0.45g, 50mL absolute ethyl alcohol are taken, it will
Its wiring solution-forming is simultaneously sufficiently stirred；Fluorescent Characterization is carried out such as to it using Fluorescence Spectrometer (LS 55, Perkin Elmer, USA)
Fig. 6.It can be seen that launch wavelength 380nm, does not have launch wavelength in red light region.
Control group 2：
Sodium hydroxide and absolute ethyl alcohol blank：50mL absolute ethyl alcohols are taken, 0.45g sodium hydroxides by its wiring solution-forming and fill
Divide stirring；Platinum electrode is inserted into, with Alternating current discharges 2h (voltage 100V).Using Fluorescence Spectrometer (LS 55, Perkin Elmer,
USA Fluorescent Characterization such as Fig. 7) is carried out to it.It can be seen that launch wavelength 475nm and 525nm, do not have transmitted wave in red light region
It is long.
Control group 3：
Indoles and absolute ethyl alcohol blank：Indoles 1.32g, 50mL absolute ethyl alcohol is taken, by its wiring solution-forming and is sufficiently stirred；It adopts
Fluorescent Characterization such as Fig. 8 is carried out to it with Fluorescence Spectrometer (LS 55, Perkin Elmer, USA).It can be seen that it is not adding in
Alkali, to the carbon dots launch wavelength that indoles-ethanol system discharges in 430nm, blue light-emitting does not have transmitted wave in red light region
It is long.
Embodiment 3：Indoles is selected to take indoles 1.32g for carbon source, takes 50mL absolute ethyl alcohols, 0.9g sodium hydroxides are inserted into platinum
Electrode with Alternating current discharges 3.5h (voltage 2200V), takes upper solution, obtains feux rouges carbon quantum dot solution.
Embodiment 4：Indoles is selected to take indoles 2g for carbon source, takes 50mL absolute ethyl alcohols, 0.45g sodium hydroxides, insertion platinum electricity
Pole with Alternating current discharges 3.5h (voltage 2640V), takes upper solution, obtains feux rouges carbon quantum dot solution.
Embodiment 5：Indoles is selected as carbon source, indoles 1.32g, takes 50mL methanol, 0.45g sodium hydroxides, is inserted into platinum electrode,
With Alternating current discharges 3.5h (voltage 2200V), upper solution is taken, obtains feux rouges carbon quantum dot solution；Using Fluorescence Spectrometer (LS
55, Perkin Elmer, USA) Fluorescent Characterization such as Fig. 9, the position of maximum excitation wavelength are carried out to prepared feux rouges carbon quantum dot
At 360nm and 540nm, corresponding optimal launch wavelength 450nm and 610nm), as can be seen from the figure this fluorescent carbon point is double
Launch wavelength, and launch wavelength will not change as excitation wavelength changes.
Embodiment 6：Ethyl alcohol is selected as carbon source, takes 50mL absolute ethyl alcohols, 0.45g sodium hydroxides are inserted into platinum electrode, use direct current
Discharge of electricity 1h (voltage 60V), takes upper solution, obtains feux rouges carbon quantum dot solution；With Fluorescence Spectrometer (LS 55, Perkin
Elmer, USA) it is as shown in Figure 10 to prepared feux rouges carbon dots progress Fluorescent Characterization.Optimal excitation peak is located at 560nm, corresponds to
Optimal launch wavelength 610nm, and launch wavelength not with excitation wavelength change and change.Illustration left figure is red carbon quantum in figure
Picture of the point solution under natural lamp, illustration right figure is the photo under 532nm green lights, from figure this it appears that prepared
Carbon dots solution send feux rouges.Transmission electron microscope picture (TEM-FEI, Tecnai G2, USA) such as Figure 10, size are mainly distributed on 3-
5nm。
Embodiment 7：Indoles is selected as carbon source, weighs 1.32g indoles, 0.45g sodium hydroxides, 50mL absolute methanols, insertion
Platinum electrode with Alternating current discharges 3.5h (voltage 2200V), takes upper solution, obtains feux rouges carbon quantum dot solution；Using fluorescence light
Spectrometer (LS 55, Perkin Elmer, USA) carries out Fluorescent Characterization to prepared feux rouges carbon quantum dot, as shown in figure 11.
Embodiment 8：Indoles is selected to take indoles 4.5g for carbon source, takes 50mL absolute ethyl alcohols, 0.45g sodium hydroxides are inserted into platinum
Electrode with Alternating current discharges 3.5h (voltage 2200V), takes upper solution, obtains feux rouges carbon quantum dot solution.
Claims (10)
1. a kind of preparation method of the carbon quantum dot to glow, it is characterised in that comprise the following steps：
1) solid base rear addition carbon source to be dissolved is added in organic solvent；
2) by metal electrode inserting step 1) in acquired solution, with direct current or Alternating current discharges, reaction in whipping process
15min-6h；
3) reaction solution is subjected to separation and purification treatment, obtains carbon quantum dot solution.
2. the preparation method of the carbon quantum dot according to claim 1 to glow, it is characterised in that：Carbon source in step 1)
For benzene ring substance or alcohols.
3. the preparation method of the carbon quantum dot according to claim 1 to glow, it is characterised in that：The metal electrode is
Platinum electrode.
4. the preparation method of the carbon quantum dot according to claim 1 to glow, it is characterised in that：The organic solvent is
Methanol or ethyl alcohol.
5. the preparation method of the carbon quantum dot according to claim 1 to glow, it is characterised in that：The solid base is hydrogen
Sodium oxide molybdena or potassium hydroxide.
6. according to the preparation method of any carbon quantum dot to glow of claim 1-5, it is characterised in that：It is described solid
Body alkali and the mass ratio of carbon source are (0.1-0.7)：1.
7. the preparation method of the carbon quantum dot according to claim 6 to glow, it is characterised in that：Alternating current discharge voltage is
2200V-2640V, DC disruptive voltage 40V-60V.
8. the preparation method of feux rouges carbon quantum dot according to claim 7, it is characterised in that：Step 4) is further included by carbon amounts
Son point solution carries out rotary evaporation and obtains feux rouges carbon quantum dot solid powder.
9. the preparation method of the carbon quantum dot of feux rouges according to claim 8, it is characterised in that：Step 3) isolates and purifies
Specially：The precipitation of reaction solution bottom is removed, gained supernatant is feux rouges carbon quantum dot solution.
10. the preparation method of the carbon quantum dot of feux rouges according to claim 8, it is characterised in that：The carbon source is indoles.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109988570A (en) * | 2019-01-28 | 2019-07-09 | 华中科技大学 | A kind of preparation facilities and preparation method of carbon quantum dot |
| CN111748344A (en) * | 2020-07-20 | 2020-10-09 | 西南大学 | Synthesis method of full-color fluorescent carbon dots, and product and application thereof |
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| CN111748344A (en) * | 2020-07-20 | 2020-10-09 | 西南大学 | Synthesis method of full-color fluorescent carbon dots, and product and application thereof |
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Effective date of registration: 20201223 Address after: 201114 room 1017, building 1, 199 JiangKai Road, Minhang District, Shanghai Patentee after: Star purple (Shanghai) new material technology development Co.,Ltd. Address before: No. 58, middle Yanta Road, Yanta District, Xi'an City, Shaanxi Province Patentee before: XI'AN University OF SCIENCE AND TECHNOLOGY |