CN104449694B - A kind of preparation method of near-infrared fluorescent carbon quantum dot - Google Patents
A kind of preparation method of near-infrared fluorescent carbon quantum dot Download PDFInfo
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- CN104449694B CN104449694B CN201410711903.0A CN201410711903A CN104449694B CN 104449694 B CN104449694 B CN 104449694B CN 201410711903 A CN201410711903 A CN 201410711903A CN 104449694 B CN104449694 B CN 104449694B
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Abstract
The preparation method that the invention discloses a kind of near-infrared fluorescent carbon quantum dot.Concrete preparation method is: a certain amount of Rhizoma Dioscoreae Zingiberensis is extracted residue and joins in secondary water, heated and stirred dispersion 20min in 100 DEG C of boiling water baths, it is added thereto to a certain amount of tellurium cadmium sulfide, cysteine and tartaric acid, it is sufficiently mixed uniformly, proceed in hydrothermal reaction kettle, 140～220 DEG C of temperature ranges, under the differential responses time, obtain the near-infrared luminous carbon quantum dot of different wave length.Raw material simplicity used in the present invention is easy to get, and only directly need to mix according to certain proportioning, and therefore experimentation is simple to operate, and experimental repeatability is higher, obtained carbon quantum dot stable performance.
Description
Technical field
The present invention relates to composite Nano micro crystal material technical field, the preparation method being specifically related to a kind of near-infrared fluorescent carbon quantum dot.
Background technology
Carbon quantum dot is compared with other carbon nanomaterial, and carbon quantum dot has the luminosity of uniqueness.The luminescence of carbon quantum dot has size and wavelength dependency.And luminescence has high stability, without photobleaching, overcome organic dyestuff luminescence unstable, the shortcoming of easy photobleaching.Carbon quantum dot is easily prepared, and the raw material that preparation uses is cheap, extensive.Additionally, carbon quantum dot low toxicity, the bio-compatibility having had, overcome inorganic-quantum-dot height poison, be unfavorable for the shortcoming applied in vivo.Owing to carbon quantum dot possesses above plurality of advantages, since being found, just of great interest.So far, potential using value is shown at bio-imaging, fluorescence sense, organic photovoltaic, light emitting diode and catalytic field.
The preparation method of current fluorescent carbon quantum dot mainly has electrochemical oxidation process, strong acid oxidizing process, high temperature pyrolytic cracking (HTP), microwave thermal solution and laser plasma method of stripping, the carbon precursor adopted mainly has (typical bibliographical information: the XuJ such as graphite, CNT, activated carbon, wax candle ash and organic carbon source, SahuS, CaoL, etal.Carbonnanoparticlesaschromophoresforphotoharvesting andphotoconversion.ChemPhysChem, 2011,12 (18): 3604-3608；HuSL, DongYG, YangJL, etal.Simultaneoussynthesisofluminescentcarbonnanoparticl esandcarbonnanocagesbylaserablationofcarbonblacksuspensi onandtheiropticallimitingproperties.JMaterChem, 2012,22:1957-1961；LongYM, ZhouCH, ZhangZL, etal.Shiftingandnon-shiftingfluorescenceemittedbycarbonn anodots.JMaterChem, 2012,22:5917-5920；F.Wang, etal., Adv.Funct.Mater.2011,21,1027；Q.Wangetal., Carbon2011,49,3134；J.Wangetal., S.Chen, Angew.Chem.2012,124,9431；ZhaiXY, ZhangP, LiuCJ, etal.Highlyluminescentcarbonnanodotsbymicrowave-assisted pyrolysis.ChemCommun, 2012,48:7955-7957).
Costly, preparation process is loaded down with trivial details and post processing is complex, and prepared fluorescent carbon quantum dot is greatly all in visible region, limits the application of carbon quantum dot for the raw material of said method employing and the instrument of use.Compared with visible light active quantum dots, near-infrared quantum dots has the advantage of uniqueness, as tissue penetration depths is relatively big, the defect etc. that visible light active quantum dots is easily disturbed when carrying out deep tissues imaging can be overcome, therefore attract wide attention in molecular biology, cytobiology and medical diagnostics etc..Therefore, the preparation method of the near-infrared carbon quantum dot that development is simple effectively, safety is cheap is particularly necessary.
Summary of the invention
A kind of method that it is an object of the invention to provide simple operation, prepare quick near-infrared fluorescent carbon quantum dot.
The technical scheme is that
The preparation method of a kind of near-infrared fluorescent carbon quantum dot, comprises the steps:
(1) weighing a certain amount of Rhizoma Dioscoreae Zingiberensis and extract residue, add secondary water, heated and stirred dispersion 20min in 100 DEG C of boiling water baths, as carbon source；
(2) in (1), add the tellurium cadmium sulfide of certain volume, then be added thereto to a certain amount of cysteine and tartaric acid, be sufficiently mixed uniformly；
(3) being poured into by step (2) gained mixed solution and carry out hydro-thermal reaction in hydrothermal reaction kettle, reaction temperature is 140～220 DEG C, and the time is 0.5～4 hour, and reaction is filtered after terminating, and obtains near-infrared fluorescent carbon quantum dot.
The preparation method of above-mentioned near-infrared fluorescent carbon quantum dot, it is 0.5～1:0.02～0.04:0.05～0.1 that described Rhizoma Dioscoreae Zingiberensis extracts residue, cysteine and tartaric mass ratio；The consumption of described tellurium cadmium sulfide is that (200～600) μ L/ (0.5～1) g Rhizoma Dioscoreae Zingiberensis extracts residue.
The beneficial effects of the present invention is:
Raw material simplicity used in the present invention is easy to get, and only directly need to mix according to certain proportioning, and therefore experimentation is simple to operate, and experimental repeatability is higher, obtained carbon quantum dot stable performance.
Accompanying drawing explanation
Fig. 1 is the excitation and emission spectra figure of carbon quantum dot prepared in embodiment 1.
Fig. 2 is the excitation and emission spectra figure of carbon quantum dot prepared in embodiment 2.
Fig. 3 is the excitation and emission spectra figure of carbon quantum dot prepared in embodiment 3.
Fig. 4 is the excitation and emission spectra figure of carbon quantum dot prepared in embodiment 4.
Fig. 5 is fluorescent carbon quantum dot emission spectrum figure under different excitation wavelengths in embodiment 3.
Detailed description of the invention
Below in conjunction with the drawings and specific embodiments, the present invention is described in further detail, but the present invention is not limited to this.
Embodiment 1
The Rhizoma Dioscoreae Zingiberensis of 0.5g is extracted in the secondary water that residue adds 40mL, heated and stirred dispersion 20min in 100 DEG C of boiling water baths, it is added thereto to the tellurium cadmium sulfide of 300 μ L, 0.02g cysteine and 0.05g tartaric acid, it is sufficiently mixed uniformly, pour in the liner of rustless steel hydrothermal reaction kettle of 50mL, set reaction temperature as 180 DEG C, react 2h.The excitation and emission spectra figure of near-infrared carbon quantum dot prepared by the present embodiment is as shown in Figure 1.
Embodiment 2
The Rhizoma Dioscoreae Zingiberensis of 1.0g is extracted in the secondary water that residue adds 40mL, heated and stirred dispersion 20min in 100 DEG C of boiling water baths, it is added thereto to the tellurium cadmium sulfide of 600 μ L, 0.04g cysteine and 0.10g tartaric acid, it is sufficiently mixed uniformly, pour in the liner of rustless steel hydrothermal reaction kettle of 50mL, set reaction temperature as 200 DEG C, react 3h.The excitation and emission spectra figure of near-infrared carbon quantum dot prepared by the present embodiment is as shown in Figure 2.
Embodiment 3
The Rhizoma Dioscoreae Zingiberensis of 0.5g is extracted in the secondary water that residue adds 40mL, heated and stirred dispersion 20min in 100 DEG C of boiling water baths, it is added thereto to the tellurium cadmium sulfide of 200 μ L, 0.02g cysteine and 0.10g tartaric acid, it is sufficiently mixed uniformly, pour in the liner of rustless steel hydrothermal reaction kettle of 50mL, set reaction temperature as 160 DEG C, react 4h.The excitation and emission spectra figure of near-infrared carbon quantum dot prepared by the present embodiment is as shown in Figure 3.
Embodiment 4
The Rhizoma Dioscoreae Zingiberensis of 0.5g is extracted in the secondary water that residue adds 40mL, heated and stirred dispersion 20min in 100 DEG C of boiling water baths, it is added thereto to the tellurium cadmium sulfide of 200 μ L, 0.02g cysteine and 0.10g tartaric acid, it is sufficiently mixed uniformly, pour in the liner of rustless steel hydrothermal reaction kettle of 50mL, set reaction temperature as 140 DEG C, react 0.5h.The excitation and emission spectra figure of near-infrared carbon quantum dot prepared by the present embodiment is as shown in Figure 4.Fluorescence emission wavelengths under different excitation wavelengths is as shown in Figure 5.
Claims (1)
1. the preparation method of a near-infrared fluorescent carbon quantum dot, it is characterised in that comprise the steps:
(1) weighing a certain amount of Rhizoma Dioscoreae Zingiberensis and extract residue, add secondary water, heated and stirred dispersion 20min in 100 DEG C of boiling water baths, as carbon source；
(2) in (1), add the tellurium cadmium sulfide of certain volume, then be added thereto to a certain amount of cysteine and tartaric acid, be sufficiently mixed uniformly；
(3) step (2) gained mixed solution is poured into hydrothermal reaction kettle carries out hydro-thermal reaction, obtain near-infrared fluorescent carbon quantum dot；
It is 0.5 ~ 1:0.02 ~ 0.04:0.05 ~ 0.1 that described Rhizoma Dioscoreae Zingiberensis extracts residue, cysteine and tartaric mass ratio；The consumption of described tellurium cadmium sulfide is that (200 ~ 600) μ L/ (0.5 ~ 1) g Rhizoma Dioscoreae Zingiberensis extracts residue；
The temperature of hydro-thermal reaction is 140～220 DEG C, and the time is 0.5～4 hour.
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| CN107651665A (en) * | 2017-10-27 | 2018-02-02 | 西安理工大学 | A kind of method that water-solubility fluorescent carbon quantum dot is prepared with dried peppermint leaf |
| CN108083257B (en) * | 2017-12-28 | 2021-07-30 | 湖南科技大学 | Method for preparing fluorescent carbon dots by taking chloroplasts as carbon sources |
| CN111234816B (en) * | 2020-02-21 | 2022-06-10 | 中国科学院大学 | Preparation method of tellurium-doped carbon quantum dots and dual properties of consumption and generation of active oxygen of tellurium-doped carbon quantum dots |
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| CN103592268A (en) * | 2013-10-31 | 2014-02-19 | 中国科学院长春光学精密机械与物理研究所 | Application of fluorescence inner filter effect based carbon nano point |
| CN103756675A (en) * | 2014-01-17 | 2014-04-30 | 西安亚博生物技术有限公司 | Nitrogen doped carbon quantum dot as well as preparation method and application thereof |
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| CN103756675A (en) * | 2014-01-17 | 2014-04-30 | 西安亚博生物技术有限公司 | Nitrogen doped carbon quantum dot as well as preparation method and application thereof |
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