CN104555978B - The preparation method of a kind of photoluminescence carbon quantum dot - Google Patents
The preparation method of a kind of photoluminescence carbon quantum dot Download PDFInfo
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- CN104555978B CN104555978B CN201310487328.6A CN201310487328A CN104555978B CN 104555978 B CN104555978 B CN 104555978B CN 201310487328 A CN201310487328 A CN 201310487328A CN 104555978 B CN104555978 B CN 104555978B
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Abstract
The present invention relates to chemistry and field of nanometer material technology, refer more particularly to the preparation method of a kind of photoluminescence carbon quantum dot. Milk and deionized water are mixed evenly by the present invention with arbitrary proportion, are then placed in baking oven in reactor and carry out hydro-thermal reaction, take out reactor and be cooled to room temperature after having reacted, obtain the aqueous dispersion system of brown color; Leave standstill, get the supernatant liquor containing photoluminescence carbon quantum dot and carry out centrifugation, with deionized water wash gained solid, obtain the aqueous solution containing the evenly photoluminescence carbon quantum dot of dispersion. The present invention has simple to operate, environmental protection, and the photoluminescence carbon quantum dot obtained can extensively for fields such as nanotechnology, medicament transport, biological detection, opto-electronic conversion and catalysis.
Description
Technical field
The present invention relates to chemistry and field of nanometer material technology, refer more particularly to the preparation method of a kind of photoluminescence carbon quantum dot.
Background technology
Owing to having unique surface effects, 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 Materials science research. Carbon nanomaterial such as soccerballene, carbon nanotube and Graphene etc. become the focus (ShaojunGuoandShaojunDong.Graphenenanosheet:synthesis of nano science research in recent years because it has various unique character, molecularengineering, thinfilm, hybrids, andenergyandanalyticalapplications.Chem.Soc.Rev., 2011,40,2644-2672). Carbon quantum dot (Carbondots, CDs) in recent years, and become research focus new in the field such as bio-sensing and imaging. Photoluminescence 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, document report a large amount of synthesis carbon quantum dot synthetic method (Wang Fu. the synthesis of luminous carbon quantum dot and application. graduate school of Chinese Academy of Sciences doctorate paper .2011.5), be divided into from top to bottom and bottom-to-top method. Top-to-bottom method comprises arc-over, laser cutting, electrochemical oxidation etc., is characterized in that utilizing the methods such as chemistry or physics to be peeled off by carbon material is carbon nano-particle, improves its luminous efficiency through further finishing; Bottom-to-top method comprises organism thermolysis, template and hydrothermal method etc., has simple to operate, and the quantum dot obtained is amorphous, and quantum yield is low.
Summary of the invention
What it is an object of the invention to provide a kind of simple to operate, environmental protection utilizes milk and deionized water, is obtained the preparation method of photoluminescence carbon quantum dot by hydrothermal method.
The preparation method of the photoluminescence carbon quantum dot of the present invention: milk and deionized water are mixed evenly with arbitrary proportion, then it is placed in baking oven in reactor to carry out hydro-thermal reaction, take out reactor after having reacted and it is cooled to room temperature, obtain the aqueous dispersion system of brown color; Leave standstill, get the supernatant liquor containing photoluminescence carbon quantum dot and carry out centrifugation, with deionized water wash gained solid (repeatedly centrifugation and washing can be carried out), obtain the aqueous solution containing the evenly photoluminescence carbon quantum dot of dispersion.
Described milk is mammal milk or the aqueous solution of mammal milk; Described mammal milk be selected from milk, goat milk, mare's milk etc. one or more.
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 photoluminescence carbon quantum dot obtained can extensively for fields such as nanotechnology, medicament transport, biological detection, opto-electronic conversion and catalysis. Utilizing the character of the photoluminescence carbon quantum dot that the present invention prepares by transmission electron microscope to measure, result display photoluminescence carbon quantum dot be dispersion state, and grain size distributes and is mainly 20��30 nanometers; Photoluminescence carbon quantum dot the present invention prepared carries out fluoroscopic examination, and result display wavelength is the aqueous solution that the UV-irradiation of 365 nanometers contains photoluminescence carbon quantum dot, can be observed significantly blue light; With spectrophotofluorometer, it is detected, it has been found that the emission wavelength of photoluminescence carbon quantum dot be stimulated wavelength size impact, there is multiple VISIBLE LIGHT EMISSION characteristic.
Accompanying drawing explanation
Fig. 1. the electromicroscopic photograph of the photoluminescence carbon quantum dot that the embodiment of the present invention 1 prepares.
Fig. 2. the photo of the photoluminescence carbon quantum dot that the embodiment of the present invention 1 prepares under visible ray (left figure) and wavelength are 365nm ultraviolet lamp (right figure).
Fig. 3. the fluorescence spectrum of the photoluminescence carbon quantum dot that the embodiment of the present invention 1 prepares.
Fig. 4. the ultraviolet visible absorption spectra figure of the photoluminescence carbon quantum dot that the embodiment of the present invention 1 prepares.
Embodiment
Embodiment 1.
It is that the ratio of 1:100 is mixed evenly taking volume ratio by milk and deionized water, then it is placed in baking oven in reactor to carry out hydro-thermal reaction, the temperature of hydro-thermal reaction is 150 DEG C, reacts and takes out reactor and be cooled to room temperature after 10 hours, obtains the aqueous dispersion system of brown color; Leave standstill, get the supernatant liquor containing photoluminescence carbon quantum dot and carry out centrifugation, with deionized water wash gained solid, after repeatedly centrifugation and washing, obtain the aqueous solution containing the evenly photoluminescence carbon quantum dot of dispersion.
Test result shows: carbon quantum dot is dispersion state, and grain size distribution is mainly 20��25 nanometers, as shown in Figure 1; The carbon quantum dot obtained is carried out fluoroscopic examination, and result display wavelength is the UV-irradiation carbon quantum dot aqueous solution of 365 nanometers, can be observed significantly blue light, as shown in Figure 2; With spectrophotofluorometer, it is detected, it has been found that the emission wavelength of carbon quantum dot be stimulated wavelength size impact, there is multiple VISIBLE LIGHT EMISSION characteristic, as shown in Figure 3; Ultraviolet absorption spectrum shows to have, in 283 nanometers, the narrow absorption peak that carbon quantum dot transition causes, as shown in Figure 4.
Embodiment 2.
It is that the ratio of 1:1 is mixed evenly taking volume ratio by milk and deionized water, then it is placed in baking oven in reactor to carry out hydro-thermal reaction, the temperature of hydro-thermal reaction is 170 DEG C, reacts and takes out reactor and be cooled to room temperature after 5 hours, obtains the aqueous dispersion system of brown color; Leave standstill, get the supernatant liquor containing photoluminescence carbon quantum dot and carry out centrifugation, with deionized water wash gained solid, after repeatedly centrifugation and washing, obtain the aqueous solution containing the evenly photoluminescence carbon quantum dot of dispersion.
Test result shows: carbon quantum dot is dispersion state, and grain size distribution is mainly 22��27 nanometers. The carbon quantum dot obtained is carried out fluoroscopic examination, and result display wavelength is the UV-irradiation carbon quantum dot aqueous solution of 365 nanometers, can be observed significantly blue light; With spectrophotofluorometer, it is detected, it has been found that the emission wavelength of carbon quantum dot be stimulated wavelength size impact, there is multiple VISIBLE LIGHT EMISSION characteristic; Ultraviolet absorption spectrum shows to have, in 283 nanometers, the narrow absorption peak that carbon quantum dot transition causes.
Embodiment 3.
It is that the ratio of 100:1 is mixed evenly taking volume ratio by milk and deionized water, then it is placed in baking oven in reactor to carry out hydro-thermal reaction, the temperature of hydro-thermal reaction is 190 DEG C, reacts and takes out reactor and be cooled to room temperature after 1 hour, obtains the aqueous dispersion system of brown color; Leave standstill, get the supernatant liquor containing photoluminescence carbon quantum dot and carry out centrifugation, with deionized water wash gained solid, after repeatedly centrifugation and washing, obtain the aqueous solution containing the evenly photoluminescence carbon quantum dot of dispersion.
Test result shows: carbon quantum dot is dispersion state, and grain size distribution is mainly 22��27 nanometers. The carbon quantum dot obtained is carried out fluoroscopic examination, and result display wavelength is the UV-irradiation carbon quantum dot aqueous solution of 365 nanometers, can be observed significantly blue light; With spectrophotofluorometer, it is detected, it has been found that the emission wavelength of carbon quantum dot be stimulated wavelength size impact, there is multiple VISIBLE LIGHT EMISSION characteristic; Ultraviolet absorption spectrum shows to have, in 283 nanometers, the narrow absorption peak that carbon quantum dot transition causes.
Embodiment 4.
It is that the ratio of 1:1 is mixed evenly taking volume ratio by goat milk and deionized water, then it is placed in baking oven in reactor to carry out hydro-thermal reaction, the temperature of hydro-thermal reaction is 180 DEG C, reacts and takes out reactor and be cooled to room temperature after 4 hours, obtains the aqueous dispersion system of brown color; Leave standstill, get the supernatant liquor containing photoluminescence carbon quantum dot and carry out centrifugation, with deionized water wash gained solid, after repeatedly centrifugation and washing, obtain the aqueous solution containing the evenly photoluminescence carbon quantum dot of dispersion.
Test result shows: carbon quantum dot is dispersion state, and grain size distribution is mainly 25��30 nanometers. The carbon quantum dot obtained is carried out fluoroscopic examination, and result display wavelength is the UV-irradiation carbon quantum dot aqueous solution of 365 nanometers, can be observed significantly blue light; With spectrophotofluorometer, it is detected, it has been found that the emission wavelength of carbon quantum dot be stimulated wavelength size impact, there is multiple VISIBLE LIGHT EMISSION characteristic; Ultraviolet absorption spectrum shows to have, in 283 nanometers, the narrow absorption peak that carbon quantum dot transition causes.
Embodiment 5.
It is that the ratio of 1:1 is mixed evenly taking volume ratio by mare's milk and deionized water, then it is placed in baking oven in reactor to carry out hydro-thermal reaction, the temperature of hydro-thermal reaction is 170 DEG C, reacts and takes out reactor and be cooled to room temperature after 6 hours, obtains the aqueous dispersion system of brown color; Leave standstill, get the supernatant liquor containing photoluminescence carbon quantum dot and carry out centrifugation, with deionized water wash gained solid, after repeatedly centrifugation and washing, obtain the aqueous solution containing the evenly photoluminescence carbon quantum dot of dispersion.
Test result shows: carbon quantum dot is dispersion state, and grain size distribution is mainly 22��30 nanometers. The carbon quantum dot obtained is carried out fluoroscopic examination, and result display wavelength is the UV-irradiation carbon quantum dot aqueous solution of 365 nanometers, can be observed significantly blue light; With spectrophotofluorometer, it is detected, it has been found that the emission wavelength of carbon quantum dot be stimulated wavelength size impact, there is multiple VISIBLE LIGHT EMISSION characteristic; Ultraviolet absorption spectrum shows to have, in 283 nanometers, the narrow absorption peak that carbon quantum dot transition causes.
Claims (2)
1. the preparation method of a photoluminescence carbon quantum dot, it is characterized in that: milk and deionized water are mixed evenly, then it is placed in reactor in baking oven, it is 150��200 DEG C in temperature and carries out hydro-thermal reaction 1��10 hour, take out reactor after having reacted and it is cooled to room temperature, obtain the aqueous dispersion system of brown color; Leave standstill, get the supernatant liquor containing photoluminescence carbon quantum dot and carry out centrifugation, with deionized water wash gained solid, obtain the aqueous solution containing the evenly photoluminescence carbon quantum dot of dispersion;
Described milk is mammal milk or the aqueous solution of mammal milk.
2. preparation method according to claim 1, is characterized in that: described mammal milk be selected from milk, goat milk, mare's milk one or more.
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| 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 |
| 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 |
| 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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| 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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| 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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