CN104555978A - Preparation method of photoluminescent carbon dots - Google Patents
Preparation method of photoluminescent carbon dots Download PDFInfo
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- CN104555978A CN104555978A CN201310487328.6A CN201310487328A CN104555978A CN 104555978 A CN104555978 A CN 104555978A CN 201310487328 A CN201310487328 A CN 201310487328A CN 104555978 A CN104555978 A CN 104555978A
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Abstract
The invention relates to the field of chemistry and nano materials, in particular to a preparation method of photoluminescent carbon dots. Milk and deionized water are uniformly mixed in any proportion and then are poured into a reaction kettle, the reaction kettle is placed in a drying oven, the mixture has a hydrothermal reaction, the reaction kettle is taken out and cooled to the room temperature after the reaction is completed, and a brown yellow aqueous solution disperse system is obtained; the brown yellow aqueous solution disperse system is left to stand, a supernatant containing the photoluminescent carbon dots is subjected to centrifugal separation, obtained solids are washed by deionized water, and an aqueous solution containing the uniformly dispersed photoluminescent carbon dots is obtained. The preparation method is simple to operate, green and environment-friendly, and the obtained photoluminescent carbon dots can be widely applied to the fields of a nanotechnology, drug delivery, biological detection, photovoltaic conversion and catalysis and the like.
Description
Technical field
The present invention relates to chemistry and field of nanometer material technology, refer more particularly to a kind of preparation method of luminescence generated by light carbon quantum dot.
Background technology
Owing to having unique skin effect, small-size effect, macro quanta tunnel effect and quantum confined effect, nano material shows unique performance in optical, electrical, magnetic, heat, mechanics, machinery etc., becomes the focus of material science research.Carbon nanomaterial such as fullerene, CNT and Graphene etc. to become focus (the Shaojun Guo andShaojun Dong.Graphene nanosheet:synthesis of nano science research in recent years because it has various peculiar property, molecular engineering, thin film, hybrids, and energy and analytical applications.Chem.Soc.Rev., 2011,40,2644-2672).Carbon quantum dot (Carbon dots, CDs) in recent years, and become study hotspot new in the field such as bio-sensing and imaging.Luminescence generated by light carbon quantum dot not only has the luminescent properties and small size property that are similar to conventional semiconductors quantum dot, but also has good water solubility and the advantage such as bio-toxicity is low.
So far, the bibliographical information synthetic method of a large amount of synthesis carbon quantum dot (Wang Fu. the synthesis of luminous carbon quantum dot and application. Postgraduate School, Chinese Academy of Sciences Ph.D. Dissertation .2011.5), be divided into from top to bottom and bottom-to-top method.Top-to-bottom method comprises arc discharge, laser cutting, electrochemical oxidation etc., is characterized in that utilizing the methods such as chemistry or physics to be peeled off by material with carbon element is carbon nano-particle, improves its luminous efficiency through further finishing; Bottom-to-top method comprises organic matter thermal decomposition, template and hydro-thermal method etc., and have simple to operate, the quantum dot obtained is amorphous, and quantum efficiency is low.
Summary of the invention
What the object of this invention is to provide a kind of simple to operate, environmental protection utilizes milk and deionized water, is obtained the preparation method of luminescence generated by light carbon quantum dot by hydro-thermal method.
The preparation method of luminescence generated by light carbon quantum dot of the present invention: milk and deionized water are mixed evenly with arbitrary proportion, then be placed in reactor in baking oven and carry out hydro-thermal reaction, react rear taking-up reactor and be cooled to room temperature, having obtained the aqueous dispersion system of brown color; Leave standstill, the supernatant got containing luminescence generated by light carbon quantum dot carries out centrifugation, spends deionized water gained solid (can carry out repeatedly centrifugation and washing), obtains the aqueous solution containing homodisperse luminescence generated by light carbon quantum dot.
Described milk is the aqueous solution of mammal milk or mammal milk; Described mammal milk is selected from one or more in milk, goat milk, mare's milk etc.
The temperature of described hydro-thermal reaction is 150 ~ 200 DEG C.
The time of described hydro-thermal reaction is 1 ~ 10 hour.
The present invention has simple to operate, environmental protection, and the luminescence generated by light carbon quantum dot obtained can be widely used in the fields such as nanometer technology, medicament transport, biological detection, opto-electronic conversion and catalysis.Utilize the character of transmission electron microscope to the luminescence generated by light carbon quantum dot that the present invention prepares to measure, result display light photoluminescence carbon quantum dot is dispersity, and grain size distribution is mainly 20 ~ 30 nanometers; Carry out fluoroscopic examination to the luminescence generated by light carbon quantum dot that the present invention prepares, result display wavelength is the aqueous solution that the UV-irradiation of 365 nanometers contains luminescence generated by light carbon quantum dot, can be observed obvious blue light; With sepectrophotofluorometer, it is detected, find that the emission wavelength of luminescence generated by light carbon quantum dot is stimulated the impact of wavelength size, has multiple VISIBLE LIGHT EMISSION characteristic.
Accompanying drawing explanation
Fig. 1. the electromicroscopic photograph of the luminescence generated by light carbon quantum dot that the embodiment of the present invention 1 prepares.
Fig. 2. the photo of the luminescence generated by light carbon quantum dot that the embodiment of the present invention 1 prepares under visible ray (left figure) and wavelength are 365nm uviol lamp (right figure).
Fig. 3. the fluorescence spectrum of the luminescence generated by light carbon quantum dot that the embodiment of the present invention 1 prepares.
Fig. 4. the ultraviolet visible absorption spectra figure of the luminescence generated by light carbon quantum dot that the embodiment of the present invention 1 prepares.
Detailed description of the invention
Embodiment 1.
Be that the ratio of 1:100 is mixed evenly with volume ratio by milk and deionized water, then be placed in reactor in baking oven and carry out hydro-thermal reaction, the temperature of hydro-thermal reaction is 150 DEG C, reacts and takes out reactor after 10 hours and be cooled to room temperature, obtain the aqueous dispersion system of brown color; Leave standstill, the supernatant got containing luminescence generated by light carbon quantum dot carries out centrifugation, spends deionized water gained solid, after repeatedly centrifugation and washing, obtains the aqueous solution containing homodisperse luminescence generated by light carbon quantum dot.
Test result shows: carbon quantum dot is dispersity, and grain size distribution is mainly 20 ~ 25 nanometers, as shown in Figure 1; Carry out fluoroscopic examination to the carbon quantum dot obtained, result display wavelength is the UV-irradiation carbon quantum dot aqueous solution of 365 nanometers, can be observed obvious blue light, as shown in Figure 2; With sepectrophotofluorometer, it is detected, find that the emission wavelength of carbon quantum dot is stimulated the impact of wavelength size, has multiple VISIBLE LIGHT EMISSION characteristic, as shown in Figure 3; Ultraviolet absorption spectrum shows to have in 283 nanometers the narrow absworption peak that carbon quantum dot transition causes, as shown in Figure 4.
Embodiment 2.
Be that the ratio of 1:1 is mixed evenly with volume ratio by milk and deionized water, then be placed in reactor in baking oven and carry out hydro-thermal reaction, the temperature of hydro-thermal reaction is 170 DEG C, reacts and takes out reactor after 5 hours and be cooled to room temperature, obtain the aqueous dispersion system of brown color; Leave standstill, the supernatant got containing luminescence generated by light carbon quantum dot carries out centrifugation, spends deionized water gained solid, after repeatedly centrifugation and washing, obtains the aqueous solution containing homodisperse luminescence generated by light carbon quantum dot.
Test result shows: carbon quantum dot is dispersity, and grain size distribution is mainly 22 ~ 27 nanometers.Carry out fluoroscopic examination to the carbon quantum dot obtained, result display wavelength is the UV-irradiation carbon quantum dot aqueous solution of 365 nanometers, can be observed obvious blue light; With sepectrophotofluorometer, it is detected, find that the emission wavelength of carbon quantum dot is stimulated the impact of wavelength size, has multiple VISIBLE LIGHT EMISSION characteristic; Ultraviolet absorption spectrum shows to have in 283 nanometers the narrow absworption peak that carbon quantum dot transition causes.
Embodiment 3.
Be that the ratio of 100:1 is mixed evenly with volume ratio by milk and deionized water, then be placed in reactor in baking oven and carry out hydro-thermal reaction, the temperature of hydro-thermal reaction is 190 DEG C, reacts and takes out reactor after 1 hour and be cooled to room temperature, obtain the aqueous dispersion system of brown color; Leave standstill, the supernatant got containing luminescence generated by light carbon quantum dot carries out centrifugation, spends deionized water gained solid, after repeatedly centrifugation and washing, obtains the aqueous solution containing homodisperse luminescence generated by light carbon quantum dot.
Test result shows: carbon quantum dot is dispersity, and grain size distribution is mainly 22 ~ 27 nanometers.Carry out fluoroscopic examination to the carbon quantum dot obtained, result display wavelength is the UV-irradiation carbon quantum dot aqueous solution of 365 nanometers, can be observed obvious blue light; With sepectrophotofluorometer, it is detected, find that the emission wavelength of carbon quantum dot is stimulated the impact of wavelength size, has multiple VISIBLE LIGHT EMISSION characteristic; Ultraviolet absorption spectrum shows to have in 283 nanometers the narrow absworption peak that carbon quantum dot transition causes.
Embodiment 4.
Be that the ratio of 1:1 is mixed evenly with volume ratio by goat milk and deionized water, then be placed in reactor in baking oven and carry out hydro-thermal reaction, the temperature of hydro-thermal reaction is 180 DEG C, reacts and takes out reactor after 4 hours and be cooled to room temperature, obtain the aqueous dispersion system of brown color; Leave standstill, the supernatant got containing luminescence generated by light carbon quantum dot carries out centrifugation, spends deionized water gained solid, after repeatedly centrifugation and washing, obtains the aqueous solution containing homodisperse luminescence generated by light carbon quantum dot.
Test result shows: carbon quantum dot is dispersity, and grain size distribution is mainly 25 ~ 30 nanometers.Carry out fluoroscopic examination to the carbon quantum dot obtained, result display wavelength is the UV-irradiation carbon quantum dot aqueous solution of 365 nanometers, can be observed obvious blue light; With sepectrophotofluorometer, it is detected, find that the emission wavelength of carbon quantum dot is stimulated the impact of wavelength size, has multiple VISIBLE LIGHT EMISSION characteristic; Ultraviolet absorption spectrum shows to have in 283 nanometers the narrow absworption peak that carbon quantum dot transition causes.
Embodiment 5.
Be that the ratio of 1:1 is mixed evenly with volume ratio by mare's milk and deionized water, then be placed in reactor in baking oven and carry out hydro-thermal reaction, the temperature of hydro-thermal reaction is 170 DEG C, reacts and takes out reactor after 6 hours and be cooled to room temperature, obtain the aqueous dispersion system of brown color; Leave standstill, the supernatant got containing luminescence generated by light carbon quantum dot carries out centrifugation, spends deionized water gained solid, after repeatedly centrifugation and washing, obtains the aqueous solution containing homodisperse luminescence generated by light carbon quantum dot.
Test result shows: carbon quantum dot is dispersity, and grain size distribution is mainly 22 ~ 30 nanometers.Carry out fluoroscopic examination to the carbon quantum dot obtained, result display wavelength is the UV-irradiation carbon quantum dot aqueous solution of 365 nanometers, can be observed obvious blue light; With sepectrophotofluorometer, it is detected, find that the emission wavelength of carbon quantum dot is stimulated the impact of wavelength size, has multiple VISIBLE LIGHT EMISSION characteristic; Ultraviolet absorption spectrum shows to have in 283 nanometers the narrow absworption peak that carbon quantum dot transition causes.
Claims (5)
1. the preparation method of a luminescence generated by light carbon quantum dot, it is characterized in that: milk and deionized water are mixed evenly, then be placed in reactor in baking oven and carry out hydro-thermal reaction, reacted rear taking-up reactor and be cooled to room temperature, having obtained the aqueous dispersion system of brown color; Leave standstill, the supernatant got containing luminescence generated by light carbon quantum dot carries out centrifugation, spends deionized water gained solid, obtains the aqueous solution containing homodisperse luminescence generated by light carbon quantum dot.
2. preparation method according to claim 1, is characterized in that: described milk is the aqueous solution of mammal milk or mammal milk.
3. preparation method according to claim 2, is characterized in that: described mammal milk is selected from one or more in milk, goat milk, mare's milk.
4. preparation method according to claim 1, is characterized in that: the temperature of described hydro-thermal reaction is 150 ~ 200 DEG C.
5. the preparation method according to claim 1 or 4, is characterized in that: the time of described hydro-thermal reaction is 1 ~ 10 hour.
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105152157A (en) * | 2015-09-15 | 2015-12-16 | 郑州大学 | Method for preparing solid light-emitting carbon point |
| CN105236386A (en) * | 2015-11-10 | 2016-01-13 | 东华大学 | Method for preparing carbon nanoparticles through corncob |
| CN106318390A (en) * | 2016-08-19 | 2017-01-11 | 北京化工大学 | Biomass nitrogen doped fluorescent carbon dot preparation method |
| CN107670664A (en) * | 2017-10-31 | 2018-02-09 | 云南健牛生物科技有限公司 | Titanic oxide composite photochemical catalyst system prepares and its application |
| CN108101019A (en) * | 2017-12-19 | 2018-06-01 | 重庆文理学院 | A kind of method that carbon quantum dot is prepared using expired Chinese patent drug |
| CN108314043A (en) * | 2018-03-21 | 2018-07-24 | 湘潭大学 | A kind of preparation method of richness nitrogen porous nano charcoal ball |
| CN114890406A (en) * | 2022-06-15 | 2022-08-12 | 辽宁大学 | Full-color photoluminescence carbon quantum dot and application thereof in full-color luminous composite film |
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| CN102583307A (en) * | 2012-01-17 | 2012-07-18 | 南京工业大学 | Fluorescent carbon quantum dots extracted from eggs and preparation method and application thereof |
| CN102745669A (en) * | 2012-07-18 | 2012-10-24 | 中国人民解放军军事医学科学院卫生装备研究所 | Method for preparing photoluminescence carbon quantum dot |
| CN102816567A (en) * | 2012-08-21 | 2012-12-12 | 中国人民解放军军事医学科学院卫生装备研究所 | Method for preparing high-yield carbon quantum dots |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102583307A (en) * | 2012-01-17 | 2012-07-18 | 南京工业大学 | Fluorescent carbon quantum dots extracted from eggs and preparation method and application thereof |
| CN102745669A (en) * | 2012-07-18 | 2012-10-24 | 中国人民解放军军事医学科学院卫生装备研究所 | Method for preparing photoluminescence carbon quantum dot |
| CN102816567A (en) * | 2012-08-21 | 2012-12-12 | 中国人民解放军军事医学科学院卫生装备研究所 | Method for preparing high-yield carbon quantum dots |
Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105152157A (en) * | 2015-09-15 | 2015-12-16 | 郑州大学 | Method for preparing solid light-emitting carbon point |
| CN105152157B (en) * | 2015-09-15 | 2017-04-12 | 郑州大学 | Method for preparing solid light-emitting carbon point |
| CN105236386A (en) * | 2015-11-10 | 2016-01-13 | 东华大学 | Method for preparing carbon nanoparticles through corncob |
| CN106318390A (en) * | 2016-08-19 | 2017-01-11 | 北京化工大学 | Biomass nitrogen doped fluorescent carbon dot preparation method |
| CN106318390B (en) * | 2016-08-19 | 2019-01-04 | 北京化工大学 | A kind of preparation method of biomass N doping fluorescent carbon point |
| CN107670664A (en) * | 2017-10-31 | 2018-02-09 | 云南健牛生物科技有限公司 | Titanic oxide composite photochemical catalyst system prepares and its application |
| CN108101019A (en) * | 2017-12-19 | 2018-06-01 | 重庆文理学院 | A kind of method that carbon quantum dot is prepared using expired Chinese patent drug |
| CN108314043A (en) * | 2018-03-21 | 2018-07-24 | 湘潭大学 | A kind of preparation method of richness nitrogen porous nano charcoal ball |
| CN108314043B (en) * | 2018-03-21 | 2021-06-18 | 湘潭大学 | Preparation method of nitrogen-rich microporous carbon nanospheres |
| CN114890406A (en) * | 2022-06-15 | 2022-08-12 | 辽宁大学 | Full-color photoluminescence carbon quantum dot and application thereof in full-color luminous composite film |
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