CN104449694A - Preparation method of near infrared fluorescent carbon quantum dots - Google Patents
Preparation method of near infrared fluorescent carbon quantum dots Download PDFInfo
- Publication number
- CN104449694A CN104449694A CN201410711903.0A CN201410711903A CN104449694A CN 104449694 A CN104449694 A CN 104449694A CN 201410711903 A CN201410711903 A CN 201410711903A CN 104449694 A CN104449694 A CN 104449694A
- Authority
- CN
- China
- Prior art keywords
- carbon quantum
- preparation
- quantum dot
- infrared fluorescent
- fluorescent carbon
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
Landscapes
- Luminescent Compositions (AREA)
- Investigating, Analyzing Materials By Fluorescence Or Luminescence (AREA)
- Carbon And Carbon Compounds (AREA)
Abstract
The invention discloses a preparation method of near infrared fluorescent carbon quantum dots. The preparation method specially comprises the following steps: adding a certain amount of peltate yam rhizome extraction residues into secondary water; heating, stirring and dispersing for 20 minutes in a 100 DEG C boiled water bath; adding a certain amount of tellurium cadmium sulfide, aminothiopropionic acid and tartaric acid; fully and uniformly mixing; converting into a hydrothermal reaction kettle; and obtaining the near infrared fluorescent carbon quantum dots with different wavelengths in different reaction times in a temperature range from 140 DEG C to 220 DEG C. Raw materials used in the invention are simple, convenient and easily available and are just directly mixed in a certain proportion, so that the experimental process is simple in operation and relatively high in experimental repeatability, and the prepared carbon quantum dots are stable in performance.
Description
Technical field
The present invention relates to composite Nano micro crystal material technical field, be specifically related to a kind of preparation method of near-infrared fluorescent carbon quantum dot.
Background technology
Carbon quantum dot is compared with other carbon nanomaterial, and carbon quantum dot has unique luminosity.The luminescence of carbon quantum dot has size and wavelength dependency.And luminescence has high stability, without photobleaching, overcome organic dye luminous unstable, the shortcoming of easy photobleaching.Carbon quantum dot is easily prepared, and the starting material that preparation uses are cheap, extensive.In addition, carbon quantum dot low toxicity, the bio-compatibility had, overcomes the high poison of inorganic-quantum-dot, is unfavorable for the shortcoming applied in vivo.Because carbon quantum dot possesses above plurality of advantages, since being found, just receiving and paid close attention to widely.So far, potential using value is shown at bio-imaging, fluorescence sense, organic photovoltaic, photodiode and catalytic field.
The preparation method of current fluorescent carbon quantum dot mainly contains electrochemical oxidation process, strong acid oxidation style, high temperature pyrolytic cracking (HTP), microwave thermal solution and laser-(produced)plasma method of stripping, the carbon precursor adopted mainly contains (the typical bibliographical informations: Xu J such as graphite, carbon nanotube, activated carbon, candle ash and organic carbon source, Sahu S, Cao L, et al.Carbon nanoparticles as chromophores for photo harvesting and photoconversion.ChemPhysChem, 2011,12 (18): 3604-3608; Hu S L, Dong Y G, Yang J L, et al.Simultaneous synthesis of luminescent carbon nanoparticles and carbon nanocages bylaser ablation of carbon black suspension and their optical limiting properties.J MaterChem, 2012,22:1957-1961; Long Y M, Zhou C H, Zhang Z L, et al.Shifting andnon-shifting fluorescence emitted by carbon nanodots.J Mater Chem, 2012,22:5917-5920; F.Wang, et al., Adv.Funct.Mater.2011,21,1027; Q.Wang et al., Carbon2011,49,3134; J.Wang etal., S.Chen, Angew.Chem.2012,124,9431; Zhai X Y, ZhangP, Liu C J, et al.Highly luminescent carbon nanodots by microwave-assistedpyrolysis.Chem Commun, 2012,48:7955-7957).
The instrument compare of the raw material that aforesaid method adopts and use is expensive, and preparation process is loaded down with trivial details and aftertreatment is comparatively complicated, and prepared fluorescent carbon quantum dot is mostly in visible region, limits the application of carbon quantum dot.Compared with visible light active quantum dots, near-infrared quantum dots has unique advantage, as tissue penetration depths is larger, the defect etc. be easily disturbed when visible light active quantum dots carries 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
The object of the present invention is to provide a kind of simple operation, prepare the method for near-infrared fluorescent carbon quantum dot fast.
Technical scheme of the present invention is:
A preparation method for near-infrared fluorescent carbon quantum dot, comprises the steps:
(1) take a certain amount of Rhizome of Peltate Yam and extract residue, add intermediate 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 add a certain amount of halfcystine and tartrate wherein, fully mix;
(3) poured in hydrothermal reaction kettle by step (2) gained mixing solutions and carry out hydro-thermal reaction, temperature of reaction is 140 ~ 220 DEG C, and the time is 0.5 ~ 4 hour, and reaction terminates rear filtration, 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 Rhizome of Peltate Yam extracts residue, halfcystine and tartaric mass ratio; The consumption of described tellurium cadmium sulfide is that (200 ~ 600) μ L/ (0.5 ~ 1) g Rhizome of Peltate Yam extracts residue.
Beneficial effect of the present invention is:
Raw material used in the present invention is easy to be easy to get, and only directly need mix according to certain proportioning, 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 the utilizing emitted light spectrogram of fluorescent carbon quantum dot under different excitation wavelengths in embodiment 3.
Embodiment
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 Rhizome of Peltate Yam of 0.5g is extracted residue to add in the intermediate water of 40mL, heated and stirred dispersion 20min in 100 DEG C of boiling water baths, add the tellurium cadmium sulfide of 300 μ L wherein, 0.02g halfcystine and 0.05g tartrate, it is fully mixed, pour in the liner of stainless steel hydrothermal reaction kettle of 50mL, setting temperature of reaction is 180 DEG C, reaction 2h.The excitation and emission spectra figure of near infrared carbon quantum dot prepared by the present embodiment as shown in Figure 1.
Embodiment 2
The Rhizome of Peltate Yam of 1.0g is extracted residue to add in the intermediate water of 40mL, heated and stirred dispersion 20min in 100 DEG C of boiling water baths, add the tellurium cadmium sulfide of 600 μ L wherein, 0.04g halfcystine and 0.10g tartrate, it is fully mixed, pour in the liner of stainless steel hydrothermal reaction kettle of 50mL, setting temperature of reaction is 200 DEG C, reaction 3h.The excitation and emission spectra figure of near infrared carbon quantum dot prepared by the present embodiment as shown in Figure 2.
Embodiment 3
The Rhizome of Peltate Yam of 0.5g is extracted residue to add in the intermediate water of 40mL, heated and stirred dispersion 20min in 100 DEG C of boiling water baths, add the tellurium cadmium sulfide of 200 μ L wherein, 0.02g halfcystine and 0.10g tartrate, it is fully mixed, pour in the liner of stainless steel hydrothermal reaction kettle of 50mL, setting temperature of reaction is 160 DEG C, reaction 4h.The excitation and emission spectra figure of near infrared carbon quantum dot prepared by the present embodiment as shown in Figure 3.
Embodiment 4
The Rhizome of Peltate Yam of 0.5g is extracted residue to add in the intermediate water of 40mL, heated and stirred dispersion 20min in 100 DEG C of boiling water baths, add the tellurium cadmium sulfide of 200 μ L wherein, 0.02g halfcystine and 0.10g tartrate, it is fully mixed, pour in the liner of stainless steel hydrothermal reaction kettle of 50mL, setting temperature of reaction is 140 DEG C, reaction 0.5h.The excitation and emission spectra figure of near infrared carbon quantum dot prepared by the present embodiment as shown in Figure 4.Fluorescence emission wavelengths under different excitation wavelength as shown in Figure 5.
Claims (4)
1. a preparation method for near-infrared fluorescent carbon quantum dot, is characterized in that comprising the steps:
(1) take a certain amount of Rhizome of Peltate Yam and extract residue, add intermediate 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 add a certain amount of halfcystine and tartrate wherein, fully mix;
(3) step (2) gained mixing solutions is poured in hydrothermal reaction kettle carry out hydro-thermal reaction, obtain near-infrared fluorescent carbon quantum dot.
2. the preparation method of near-infrared fluorescent carbon quantum dot according to claim 1, is characterized in that: it is 0.5 ~ 1:0.02 ~ 0.04:0.05 ~ 0.1 that described Rhizome of Peltate Yam extracts residue, halfcystine and tartaric mass ratio.
3. the preparation method of near-infrared fluorescent carbon quantum dot according to claim 1, is characterized in that: the consumption of described tellurium cadmium sulfide is (200 ~ 600) μ L/ (0.5 ~ 1) g Rhizome of Peltate Yam extraction residue.
4. the preparation method of near-infrared fluorescent carbon quantum dot according to claim 1, is characterized in that: the temperature of described hydro-thermal reaction is 140 ~ 220 DEG C, and the time is 0.5 ~ 4 hour.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410711903.0A CN104449694B (en) | 2014-11-28 | 2014-11-28 | A kind of preparation method of near-infrared fluorescent carbon quantum dot |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410711903.0A CN104449694B (en) | 2014-11-28 | 2014-11-28 | A kind of preparation method of near-infrared fluorescent carbon quantum dot |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN104449694A true CN104449694A (en) | 2015-03-25 |
| CN104449694B CN104449694B (en) | 2016-06-29 |
Family
ID=52896460
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201410711903.0A Expired - Fee Related CN104449694B (en) | 2014-11-28 | 2014-11-28 | A kind of preparation method of near-infrared fluorescent carbon quantum dot |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN104449694B (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN108083257A (en) * | 2017-12-28 | 2018-05-29 | 湖南科技大学 | A kind of method that fluorescent carbon point is prepared using chloroplaset as carbon source |
| CN111234816A (en) * | 2020-02-21 | 2020-06-05 | 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 |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20110114181A1 (en) * | 2009-11-13 | 2011-05-19 | Kim Jae-Il | Eco-friendly method of manufacturing quantum dots by using natural oil |
| 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 |
-
2014
- 2014-11-28 CN CN201410711903.0A patent/CN104449694B/en not_active Expired - Fee Related
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20110114181A1 (en) * | 2009-11-13 | 2011-05-19 | Kim Jae-Il | Eco-friendly method of manufacturing quantum dots by using natural oil |
| 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 |
Non-Patent Citations (2)
| Title |
|---|
| LEI FENG等: "A novel method for aqueous synthesis of CdTe duantum dots", 《SPECTROCHIMICA ACTA PART A: MOLECULAR AND BIOMOLECULAR SPECTROSCOPY》 * |
| LONG LI等: "Ultrasensitive electrochemiluminescence immunoassay for tumor marker based on quantum dots coated carbon nanospheres", 《JOURNAL OF LUMINESCENCE》 * |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN108083257A (en) * | 2017-12-28 | 2018-05-29 | 湖南科技大学 | A kind of method that fluorescent carbon point is prepared using chloroplaset as carbon source |
| 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 |
| CN111234816A (en) * | 2020-02-21 | 2020-06-05 | 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 |
| 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 |
Also Published As
| Publication number | Publication date |
|---|---|
| CN104449694B (en) | 2016-06-29 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| Dang et al. | Large-scale ultrasonic fabrication of white fluorescent carbon dots | |
| CN103848410B (en) | A kind of hydrothermal preparing process of fluorescent carbon quantum dot | |
| CN105647526B (en) | A kind of nearly full spectrum fluorescent nano-sized carbon point and preparation method thereof | |
| CN104030269B (en) | The preparation method of red carbon quantum dot and application | |
| CN104560035B (en) | Carbon quantum dot fluorescence labeling material with orange peels used as carbon source as well as preparation method and application of carbon quantum dot fluorescence labeling material | |
| CN105271172A (en) | Preparation method of super-high-quantum-yield carbon quantum dots with citric acid-urea as raw materials | |
| CN103387219A (en) | A preparation method for water-soluble multicolor carbon quantum points by microwave radiation | |
| CN104495782B (en) | With the method that magenta prepares near-infrared carbon quantum dot for carbon source | |
| CN104449694B (en) | A kind of preparation method of near-infrared fluorescent carbon quantum dot | |
| CN104479674B (en) | Take Xylene Brilliant Cyanine G as the method that carbon source prepares near infrared carbon quantum dot | |
| CN104388082A (en) | Environment-friendly synthetic method of orange nitrogen/sulfur codoped carbon quantum dots | |
| CN104987861A (en) | Method for preparing carbon dots with up-down conversion luminescence characteristic from maize straw | |
| CN104528684B (en) | A kind of method that under the conditions of alkalescence, carbon quantum dot is prepared in ketone carbonization | |
| CN106978170B (en) | A kind of preparation method of water-solubility fluorescent carbon quantum dot | |
| CN106629664B (en) | A kind of method and its application synthesizing carbon quantum dot using water chestnut as raw material microwave | |
| CN103897696B (en) | Nm near-infrared long-afterglow material of a kind of Cr doping and preparation method thereof | |
| CN104232091B (en) | Up-conversion nano material NaYbF4: Tm and its preparation method | |
| Rodrigues et al. | An eco-friendly green and facile synthesis of carbon dots from red propolis wax with photoluminescence dependent of reaction time and thermal treatment in solid state | |
| CN107381536B (en) | Method for rapidly preparing water-soluble fluorescent carbon quantum dots in large scale | |
| CN104004517A (en) | Method for preparing regular-morphology small-size near-infrared long-afterglow luminescent nano material | |
| CN106916588A (en) | A kind of method that Ipomoea batatas stalk prepares fluorescent carbon point | |
| CN103627394A (en) | Method for preparing beta-NaGdF4:Yb<3+>, Er<3+> upconversion fluorescence material through electro-deposition | |
| CN103724316A (en) | Preparation method and application of sesamol intermediate heliotropin | |
| CN105907391A (en) | Method for preparing carbon quantum dots by aldehyde precursor | |
| CN103305222B (en) | KSc2F7: yb, preparation method and application of Er up-conversion fluorescent nanorods |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| CF01 | Termination of patent right due to non-payment of annual fee | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20160629 Termination date: 20211128 |