CN110373184A - A kind of synthetic method of high yield red fluorescence carbon quantum dot material - Google Patents
A kind of synthetic method of high yield red fluorescence carbon quantum dot material Download PDFInfo
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- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 title claims abstract description 52
- 239000000463 material Substances 0.000 title claims abstract description 28
- 238000010189 synthetic method Methods 0.000 title claims abstract description 16
- 239000000725 suspension Substances 0.000 claims abstract description 24
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims abstract description 21
- 239000000243 solution Substances 0.000 claims abstract description 21
- 238000006862 quantum yield reaction Methods 0.000 claims abstract description 16
- 239000002243 precursor Substances 0.000 claims abstract description 14
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 12
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 10
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 10
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 8
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- 238000003756 stirring Methods 0.000 claims abstract description 5
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- WMFOQBRAJBCJND-UHFFFAOYSA-M Lithium hydroxide Chemical compound [Li+].[OH-] WMFOQBRAJBCJND-UHFFFAOYSA-M 0.000 claims description 20
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid group Chemical group C(CC(O)(C(=O)O)CC(=O)O)(=O)O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims description 18
- 230000005284 excitation Effects 0.000 claims description 18
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- 229910021641 deionized water Inorganic materials 0.000 claims description 7
- 239000004202 carbamide Substances 0.000 claims description 6
- XSQUKJJJFZCRTK-UHFFFAOYSA-N urea group Chemical group NC(=O)N XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims description 6
- 238000001291 vacuum drying Methods 0.000 claims description 6
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 4
- 239000007864 aqueous solution Substances 0.000 claims description 4
- 238000001514 detection method Methods 0.000 claims description 4
- 239000002904 solvent Substances 0.000 claims description 4
- 238000005286 illumination Methods 0.000 claims description 3
- 238000000926 separation method Methods 0.000 claims description 3
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- 229910052783 alkali metal Inorganic materials 0.000 claims description 2
- 150000001340 alkali metals Chemical class 0.000 claims description 2
- 239000000908 ammonium hydroxide Substances 0.000 claims description 2
- 230000000694 effects Effects 0.000 claims description 2
- 239000002244 precipitate Substances 0.000 claims description 2
- 239000011734 sodium Substances 0.000 claims description 2
- 239000012263 liquid product Substances 0.000 claims 1
- 238000005259 measurement Methods 0.000 claims 1
- 239000002096 quantum dot Substances 0.000 claims 1
- 238000000034 method Methods 0.000 abstract description 10
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- 239000002994 raw material Substances 0.000 abstract description 3
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- 229910001413 alkali metal ion Inorganic materials 0.000 description 1
- 150000001408 amides Chemical class 0.000 description 1
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- LUMVCLJFHCTMCV-UHFFFAOYSA-M potassium;hydroxide;hydrate Chemical compound O.[OH-].[K+] LUMVCLJFHCTMCV-UHFFFAOYSA-M 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 239000000047 product Substances 0.000 description 1
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- B82Y20/00—Nanooptics, e.g. quantum optics or photonic crystals
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- H01L33/00—Semiconductor devices having potential barriers specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
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Abstract
The invention discloses a kind of synthetic methods of high yield red fluorescence carbon quantum dot material.Its synthetic method is: first weighing carbon source and nitrogen source respectively, is added in polar solvent n,N-Dimethylformamide, stirring is to being completely dissolved to obtain precursor solution；Precursor solution is transferred in polytetrafluoroethyllining lining hydrothermal reaction kettle again, at 180 DEG C of temperature, 6 hours carbonization treatments is kept the temperature, obtains suspension reaction product after cooling；It is stirred after addition alkaline solution treatment in suspension again, is centrifuged, washs, being dried to obtain red fluorescence carbon quantum dot material.The carbon quantum dot material that the present invention synthesizes can emit feux rouges in wavelength under the exciting light of 300~600nm, synthesis technology of the invention and separating-purifying process are simple, fluorescence quantum yield is high, it is repeated it is strong, raw material is cheap, is suitable for large-scale mass production.Simultaneously red fluorescence carbon quantum dot prepared by the present invention prepare white light-emitting diodes (WLED) and in terms of have broad application prospects.
Description
Technical field
The present invention relates to photoelectric display illumination and biological detection technical field of nano material, and in particular to a kind of high yield
The synthetic method of red fluorescence carbon quantum dot material.
Background technique
Quanta point material is a kind of semiconductor nano material with excellent photoluminescent property, and emission spectrum can be with its size
Change and change, light emitting region covers entire visible regime.Since its good optical property makes in photoelectric device, too
There are many applications in the fields such as positive energy battery, biomarker.
Fluorescent carbon quantum dot (CQDs) causes scientific circles as a kind of novel zero dimension c-based nanomaterial in recent years
Extensive concern, compared with traditional semiconductor-quantum-point and organic fluorescent dye, CQDs has many unique performances, including excellent
Good optical property, excellent dissolubility, good biological safety and good biological stability.
But there is also some problems at present by CQDs.For example, the best of carbon nano-particles prepared by the overwhelming majority swashs
Hair and launch wavelength are all to be located at blue-green region, and the absorption and transmitting in long wavelength region, especially red light region are but
It is weaker, this prepare bottleneck not only in biomedical applications cell and biological tissue bring serious light injury, but also
There is the defects of tissue penetration and low signal resolution；White light-emitting diodes (WLED) is prepared using CQDs, advantage exists
In can the InGaN chip based on blue light-emitting as exciting light, element without sending out ultraviolet light, to avoid ultraviolet light to people
The harm of body health.But lack effective red fluorescence CQDs base fluorescent powder at present, so that the colour developing of the WLED based on CQDs
Index is lower, and correlated colour temperature is higher, is unfavorable for that true apparent colour is presented.Although currently, there is a small number of carbon quantum dots reported
Although having red fluorescence, its fluorescence quantum yield is often below 10%, and it is very low that means of purification can be related to separative efficiency
Column chromatography and dialysis etc. technologies.Therefore, find it is a kind of simplicity, can amplifying, efficient, high quantum production rate red is glimmering
The method of light carbon quantum dot is just very crucial.Synthetic method proposed by the present invention can effectively solve the problem that above-mentioned problem.
Summary of the invention
The invention proposes a kind of synthetic method of high yield red fluorescence carbon quantum dot material, this method uses solvent heat
Carbon source and nitrogen source, are first dissolved in n,N-Dimethylformamide by the method for method and aqueous slkali post-processing, by 180 DEG C of height
Temperature carbonization forms suspension, and aqueous slkali is then added, and finally obtains red fluorescence carbon quantum after centrifugation, deionized water washing
Point material.The by-product and intermediate product of the synthetic method are few, and dialysis purification step of the obtained suspension without complexity,
Solid carbon quantum dot product can be obtained, enormously simplify preparation process, meet environmentally protective theory, and control can be passed through
Type and the concentration of aqueous slkali is added to synthesize the red fluorescence carbon quantum dot of different luminosities.
The purpose of the present invention is overcome in the prior art carbon quantum dot extent of fluorescence be concentrated mainly on blue green light region, feux rouges
The deficiency of part low yield and excitation wavelength accordance with tolerance provides a kind of synthesis side of high yield red fluorescence carbon quantum dot
Method.High yield red fluorescence carbon quantum dot material has been synthesized by the method for solvent-thermal method and aqueous slkali post-processing, has been made
Standby white light-emitting diodes (WLED) and biological detection etc. provide wide application prospect.
The invention is realized in this way.A kind of synthetic method of high yield red fluorescence carbon quantum dot material, the steps include:
A), 0.8~1.2g carbon source and 1.8~2.2g nitrogen source are weighed respectively, are added to 9~11mL solvent N, N- dimethyl methyl
In amide, stirring is to being completely dissolved to obtain precursor solution；
B), the obtained precursor solution of step a) is transferred in 25mL polytetrafluoroethyllining lining hydrothermal reaction kettle and is kept the temperature,
180 DEG C of temperature, time 6h, then cooled to room temperature obtains suspension；
C), aqueous slkali is added by suspension and aqueous slkali volume ratio 1:2 in the suspension that step b) is obtained, aqueous slkali
Molar concentration be 0.5~5mol/L, stir 2~5min, be centrifugated at 8000~15000rpm, taking precipitate addition go from
After sub- water washing, 8000~15000rpm is centrifuged again, is regathered sediment, is then obtained sediment in 60 DEG C of vacuum drying
Red fluorescence carbon quantum dot material；
By the way that the type of different aqueous slkalis is added and adjusts various concentration (0.5~5mol/L) available illumination effect
Different carbon quantum dots, absolute fluorescence quantum yield are 12.07%~34.09%.
The carbon source is citric acid；
The nitrogen source is urea；
The aqueous slkali is lithium hydroxide, sodium hydroxide, potassium hydroxide, ammonium hydroxide, preferably lithium hydroxide.
Absolute fluorescence quantum yield of the present invention is that the carbon quantum dot material of synthesis is dispersed in Diluted Alcohol solution (volume
Score 50.5%) in measured by liquid integrating sphere.
It is Li in the corresponding absolute fluorescence quantum yield of the different alkali metal solns of same concentration (1.25mol/L)+----
34.09% > Na+--- -29.29% > K+--- -27.64%.
High yield red fluorescence carbon quantum dot material prepared by the present invention, fluorescence quantum yield is high, and has preferable
Thermal stability.
The present invention has excitation wavelength compared to the carbon quantum dot that hydro-thermal method synthesizes, the red fluorescence carbon quantum dot of preparation
No dependence, under the exciting light irradiation of different wave length of the same sample within the scope of 300~600nm, fluorescence peak position is basic
It will not change, there is excitation wavelength no dependence.
Report, using the carbon quantum dot material of same raw material and same solvent structure, there is exciting light at present
Wavelength accordance with tolerance, and have multiple glow peaks in visible light region.Influence due to alkaline environment to carbon quantum dot surface electronic state
And alkali metal ion can improve the fermi level of carbon quantum dot, the fluorescence of carbon quantum dot prepared by the present invention is in red light region
Single glow peak and surface metal Li+The carbon quantum dot absolute fluorescence quantum yield highest of modification.
Red fluorescence carbon quantum dot material prepared by the present invention is preparing white light-emitting diodes (WLED) and biological detection side
Mask has broad application prospects.
In the present invention, alkaline solution treatment only need to be added after obtaining suspension, after centrifugation, deionized water washing
It is dry, red fluorescence carbon quantum dot solid product can be obtained, need without traditional carbon quantum dot method of purification by for a long time
The complex separations steps such as dialysis, freeze-drying, chromatography post separation.By-product and intermediate product of the invention is few, experiment is repeatable
Property is strong, easy to operate, raw material dosage is few, fluorescence quantum yield is high, is suitable for large-scale mass production.
Detailed description of the invention
Fig. 1 is that reaction temperature is 180 DEG C in embodiment 1, reaction time 6h, and added aqueous slkali is 1.25mol/L LiOH institute
The luorescence excitation spectrogram and transmitting spectrogram obtained；
Fig. 2 is that reaction temperature is 180 DEG C in embodiment 1, reaction time 6h, when added aqueous slkali is 1.25mol/L LiOH
Fluorescence emission spectrogram of compound under corresponding difference excitation wavelength；
Fig. 3 is that reaction temperature is 180 DEG C in embodiment 2, reaction time 6h, and added aqueous slkali is 1.25mol/L KOH institute
The luorescence excitation spectrogram and transmitting spectrogram obtained；
Fig. 4 is that reaction temperature is 180 DEG C in embodiment 3, reaction time 6h, and added aqueous slkali is 0.75mol/L NaOH institute
The luorescence excitation spectrogram and transmitting spectrogram obtained；
Fig. 5 is that reaction temperature is 180 DEG C in embodiment 3, reaction time 6h, when added aqueous slkali is 0.75mol/L NaOH
Fluorescence emission spectrogram of compound under corresponding difference excitation wavelength；
Fig. 6 is that reaction temperature is 180 DEG C in embodiment 4, reaction time 6h, and added aqueous slkali is 1.25mol/L NaOH institute
The luorescence excitation spectrogram and transmitting spectrogram obtained；
Specific embodiment
With embodiment, the present invention is further described below.
Embodiment 1:
A kind of synthetic method of high yield red fluorescence carbon quantum dot material, it is characterised in that the following steps are included:
A), 1g citric acid and 2g urea are weighed respectively, is added in 10mL n,N-Dimethylformamide, are stirred to complete
Dissolution obtains precursor solution；
B), the obtained precursor solution of step a) is transferred in 25mL polytetrafluoroethyllining lining hydrothermal reaction kettle and is kept the temperature,
180 DEG C of temperature, time 6h, then cooled to room temperature obtains suspension；
C), 1.25mol/L LiOH is added by suspension and aqueous slkali volume ratio 1:2 in the suspension that step b) is obtained
Aqueous solution is stirred two minutes, is centrifugated at 13000rpm, and 13000rpm is centrifuged after taking precipitating that deionized water washing is added,
Sediment is collected, then 60 DEG C of vacuum drying obtain red fluorescence carbon quantum dot.
Red fluorescence carbon quantum dot manufactured in the present embodiment, referring to Fig. 1, solid line is that launch wavelength is 611nm corresponding sharp
Spectrogram is sent out, dotted line is that excitation wavelength is the corresponding transmitting spectrogram of 550nm；Referring to fig. 2, with the change of excitation wavelength, carbon amounts
The glow peak position of son point does not change substantially, shows as excitation wavelength independence；It is measured with liquid integrating sphere in dilute second
Absolute fluorescence quantum yield in alcoholic solution (volume fraction 50.5%) is 34.09%.
Embodiment 2:
A kind of synthetic method of high yield red fluorescence carbon quantum dot material, it is characterised in that the following steps are included:
A), 1g citric acid and 2g urea are weighed respectively, is added in 10mL n,N-Dimethylformamide, are stirred to complete
Dissolution obtains precursor solution；
B), the obtained precursor solution of step a) is transferred in 25mL polytetrafluoroethyllining lining hydrothermal reaction kettle and is kept the temperature,
180 DEG C of temperature, time 6h, then cooled to room temperature obtains suspension；
C), 1.25mol/L KOH water is added by suspension and aqueous slkali volume ratio 1:2 in the suspension that step b) is obtained
Solution is stirred two minutes, is centrifugated at 13000rpm, and 13000rpm is centrifuged after taking precipitating that deionized water washing is added, and is received
Collect sediment, then 60 DEG C of vacuum drying obtain red fluorescence carbon quantum dot.
Red fluorescence carbon quantum dot manufactured in the present embodiment, referring to Fig. 3, solid line is that launch wavelength is 611nm corresponding sharp
Spectrogram is sent out, dotted line is that excitation wavelength is the corresponding transmitting spectrogram of 548nm；It is measured with liquid integrating sphere in Diluted Alcohol solution (volume
Score 50.5%) in absolute fluorescence quantum yield be 27.64%.
Embodiment 3:
A kind of synthetic method of high yield red fluorescence carbon quantum dot material, it is characterised in that the following steps are included:
A), 1g citric acid and 2g urea are weighed respectively, is added in 10mL n,N-Dimethylformamide, are stirred to complete
Dissolution obtains precursor solution；
B), the obtained precursor solution of step a) is transferred in 25mL polytetrafluoroethyllining lining hydrothermal reaction kettle and is kept the temperature,
180 DEG C of temperature, time 6h, then cooled to room temperature obtains suspension；
C), 0.75mol/L NaOH is added by suspension and aqueous slkali volume ratio 1:2 in the suspension that step b) is obtained
Aqueous solution is stirred two minutes, is centrifugated at 13000rpm, and 13000rpm is centrifuged after taking precipitating that deionized water washing is added,
Sediment is collected, then 60 DEG C of vacuum drying obtain red fluorescence carbon quantum dot.
Red fluorescence carbon quantum dot manufactured in the present embodiment, referring to fig. 4, solid line are that launch wavelength is 610nm corresponding sharp
Spectrogram is sent out, dotted line is that excitation wavelength is the corresponding transmitting spectrogram of 546nm；Referring to Fig. 5, with the change of excitation wavelength, carbon amounts
The glow peak position of son point does not change substantially, shows as excitation wavelength independence；It is measured with liquid integrating sphere in dilute second
Absolute fluorescence quantum yield in alcoholic solution (volume fraction 50.5%) is 15.07%.
Embodiment 4:
A kind of synthetic method of high yield red fluorescence carbon quantum dot material, it is characterised in that the following steps are included:
A), 1g citric acid and 2g urea are weighed respectively, is added in 10mL n,N-Dimethylformamide, are stirred to complete
Dissolution obtains precursor solution；
B), the obtained precursor solution of step a) is transferred in 25mL polytetrafluoroethyllining lining hydrothermal reaction kettle and is kept the temperature,
180 DEG C of temperature, time 6h, then cooled to room temperature obtains suspension；
C), 1.25mol/L NaOH is added by suspension and aqueous slkali volume ratio 1:2 in the suspension that step b) is obtained
Aqueous solution is stirred two minutes, is centrifugated at 13000rpm, and 13000rpm is centrifuged after taking precipitating that deionized water washing is added,
Sediment is collected, then 60 DEG C of vacuum drying obtain red fluorescence carbon quantum dot.
Red fluorescence carbon quantum dot manufactured in the present embodiment, referring to Fig. 6, solid line is that launch wavelength is 610nm corresponding sharp
Spectrogram is sent out, dotted line is that excitation wavelength is the corresponding transmitting spectrogram of 548nm；It is measured with liquid integrating sphere in Diluted Alcohol solution (volume
Score 50.5%) in absolute fluorescence quantum yield be 29.29%.
Claims (5)
1. a kind of synthetic method of high yield red fluorescence carbon quantum dot material, it is characterised in that the following steps are included:
A), 0.8~1.2g carbon source and 1.8~2.2g nitrogen source are weighed respectively, are added to 9~11mL solvent n,N-Dimethylformamide
In, stirring is to being completely dissolved to obtain precursor solution；
B), the obtained precursor solution of step a) is transferred in 25mL polytetrafluoroethyllining lining hydrothermal reaction kettle and is kept the temperature, temperature
180 DEG C, time 6h, then cooled to room temperature obtains suspension；
C), aqueous slkali, mole of aqueous slkali is added by suspension and aqueous slkali volume ratio 1:2 in the suspension that step b) is obtained
Concentration is 0.5~5mol/L, stirs 2~5min, is centrifugated at 8000~15000rpm, and deionized water is added in taking precipitate
After washing, 8000~15000rpm is centrifuged again, regathers sediment, sediment is then obtained red in 60 DEG C of vacuum drying
Fluorescent carbon quantum dot material；
The different carbon of illumination effect can be obtained by addition variety classes aqueous slkali, and adjusting 0.5~5mol/L of various concentration
Quantum dot, absolute fluorescence quantum yield are 12.07%~34.09%.
The carbon source is citric acid；
The nitrogen source is urea；
The aqueous slkali is lithium hydroxide, sodium hydroxide, potassium hydroxide, ammonium hydroxide, preferably lithium hydroxide.
2. a kind of synthetic method of high yield red fluorescence carbon quantum dot material according to claim 1, it is characterised in that
Absolute fluorescence quantum yield is that the carbon quantum dot of synthesis is dispersed in Diluted Alcohol solution (volume fraction 50.5%) through liquid product
Bulb separation measurement.
3. a kind of synthetic method of high yield red fluorescence carbon quantum dot material according to claim 1, it is characterised in that
The carbon quantum dot that addition LiOH aqueous solution obtains in suspension in step c) is compared to other aqueous slkali absolute fluorescence quantum yields
Highest, the corresponding absolute fluorescence quantum yield of the different alkali metal solns of same concentration (1.25mol/L) is Li+--- -34.09%
> Na+--- -29.29% > K+--- -27.64%.
4. a kind of high yield red fluorescence carbon quantum dot material according to claim 1, it is characterised in that the material is adopted
When being irradiated with the exciting light (300~600nm) of different wave length, red of the equal emission wavelength peak in 610~630nm or so is glimmering
Light has excitation wavelength no dependence.
5. a kind of application of high yield red fluorescence carbon quantum dot material according to claim 1, it is characterised in that red
Fluorescent carbon quantum dot material has broad application prospects in terms of preparing white light-emitting diodes (WLED) and biological detection.
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Cited By (5)
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|---|---|---|---|---|
| CN110980690A (en) * | 2019-12-24 | 2020-04-10 | 云南大学 | Method for preparing narrow-band red fluorescent carbon quantum dots by using titanyl phthalocyanine |
| CN111504971A (en) * | 2020-05-11 | 2020-08-07 | 吉林大学 | 2, 4-dichlorphenoxyacetic acid on-site quantitative detection platform based on integration of target response type 3D printing model and smart phone |
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| CN116948640A (en) * | 2023-07-27 | 2023-10-27 | 云南大学 | Method for preparing green light carbon quantum dots with ultrahigh fluorescence quantum yield by one-step hydrothermal method and application |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110980690A (en) * | 2019-12-24 | 2020-04-10 | 云南大学 | Method for preparing narrow-band red fluorescent carbon quantum dots by using titanyl phthalocyanine |
| CN110980690B (en) * | 2019-12-24 | 2023-03-28 | 云南大学 | Method for preparing narrow-band red fluorescent carbon quantum dots by using titanyl phthalocyanine |
| CN111504971A (en) * | 2020-05-11 | 2020-08-07 | 吉林大学 | 2, 4-dichlorphenoxyacetic acid on-site quantitative detection platform based on integration of target response type 3D printing model and smart phone |
| CN114455567A (en) * | 2020-11-03 | 2022-05-10 | 广东量子墨滴生物科技有限公司 | Preparation method and application of carbon nanoparticles |
| CN114455567B (en) * | 2020-11-03 | 2023-06-30 | 广东量子墨滴生物科技有限公司 | Preparation method and application of carbon nano particles |
| CN115125000A (en) * | 2022-07-06 | 2022-09-30 | 重庆国科医创科技发展有限公司 | Preparation method of red light emission carbon quantum dot and application of carbon quantum dot |
| CN115125000B (en) * | 2022-07-06 | 2023-11-03 | 重庆国科医创科技发展有限公司 | Preparation method of red light emission carbon quantum dot and application of carbon quantum dot |
| CN116948640A (en) * | 2023-07-27 | 2023-10-27 | 云南大学 | Method for preparing green light carbon quantum dots with ultrahigh fluorescence quantum yield by one-step hydrothermal method and application |
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