CN107163935A - A kind of method for synthesizing full light carbon point and its carbon point application - Google Patents
A kind of method for synthesizing full light carbon point and its carbon point application Download PDFInfo
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- CN107163935A CN107163935A CN201710441428.3A CN201710441428A CN107163935A CN 107163935 A CN107163935 A CN 107163935A CN 201710441428 A CN201710441428 A CN 201710441428A CN 107163935 A CN107163935 A CN 107163935A
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
- C09K11/08—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials
- C09K11/65—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing carbon
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y20/00—Nanooptics, e.g. quantum optics or photonic crystals
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
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- C—CHEMISTRY; METALLURGY
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- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B33/00—Silicon; Compounds thereof
- C01B33/113—Silicon oxides; Hydrates thereof
- C01B33/12—Silica; Hydrates thereof, e.g. lepidoic silicic acid
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- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
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- C01P2002/80—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/80—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70
- C01P2002/84—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70 by UV- or VIS- data
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/80—Particles consisting of a mixture of two or more inorganic phases
Abstract
The invention discloses a kind of method for synthesizing full light carbon point and its carbon point application.Comprise the following steps：Carbon source and passivator and ammoniacal liquor are put into solvent in the lump, 3 ~ 8 hours are reacted at 80 ~ 110 DEG C to synthesize full light carbon point, obtain the carbon dots solution containing full light carbon point of claret, passivator and the mass ratio of carbon source are 0.1 ~ 0.7, ammoniacal liquor and the mass ratio of carbon source are 5 ~ 30, solvent and the mass ratio of carbon source are 25 ~ 100, and carbon source is ammonium citrate；Passivator is ethylenediamine tetra-acetic acid；Solvent is DMF or deionized water.It is of the invention simple efficient, solvent-thermal method is used using ammonium citrate as carbon source, EDTA is passivator, ammoniacal liquor is that reaction medium one-step synthesis goes out under the irradiation of 365 nano-ultraviolet lights to show full light carbon point.This method prepares carbon point raw material inexpensively, and step is simple, and mild condition is controllable, and the carbon point luminous intensity prepared is high, and stability is good.
Description
Technical field
The present invention relates to the preparation method of carbon nanomaterial, specifically refer to be related to a kind of method for synthesizing full light carbon point and its
Carbon point application.
Background technology
Carbon point（CarbonDots,CDs）It is the quasi- ball-type carbon nano-particles that a kind of diameter is less than 10 nanometers.Carbon point is because of it
With fluorescent stabilization is high, resistance to photobleaching and without optical flare, excitation wavelength and launch wavelength are tunable, good biocompatibility, toxicity
Low excellent performance and the concern for enjoying numerous researchers.Therefore, carbon point can be used as semiconductor-quantum-point（Such as CdS,
CdSe, CdTe etc.）With the substitute of organic dyestuff and be applied to the neck such as biomarker, bio-imaging, catalysis and photoelectric device
Domain.
At present, the carbon point of synthesis is the photoluminescence property with blue light mostly, and due to the cell or group of organism
Knit the area for being unfavorable for target signal and background signal when these carbon points are used for into cell imaging with stronger autologous blue-fluorescence
Point, ambient interferences are larger, and lack the carbon point lighted in full optical range.Therefore, be highly desirable to find it is a kind of simple, with honest and clean
The method that the raw material of valency is carbon source to synthesize the carbon point of other glow colors, solves vacancy of the carbon point in other glow colors.
The content of the invention
The invention aims to overcome the shortcoming and defect that prior art is present, and it is simple to provide a kind of synthetic method
Effectively, raw material is cheap and easy to get, the method for the gentle and environment-friendly full light carbon point of synthesis of reaction condition.The carbon point of the synthesis is molten
In liquid, under portable 365 nanometers of ultra violet lamps, the carbon dots solution that synthesizes present it is bright it is red, orange, yellow, white, blue or green, blue,
Bluish violet.
Second object of the present invention is to provide the application of the carbon point synthesized by the above method.
To realize first goal of the invention of the present invention, its technical scheme is that the method for synthesizing full light carbon point includes following step
Suddenly：
Carbon source and passivator and ammoniacal liquor are put into solvent in the lump, 3 ~ 8 hours are reacted at 80 ~ 110 DEG C to synthesize full light carbon point,
Obtain the carbon dots solution containing full light carbon point of claret, the mass ratio of passivator and carbon source is 0.1 ~ 0.7, ammoniacal liquor and carbon source
Mass ratio is 5 ~ 30, and the mass ratio of solvent and carbon source is 25 ~ 100, and carbon source is ammonium citrate；Passivator is ethylenediamine tetra-acetic acid；
Solvent is DMF or deionized water.The carbon dots solution of claret rubescent, orange, yellow, white, the blue or green, blueness under uviol lamp is obtained, is presented
Full spectrum fluorescent characteristic.
The present invention also provide it is a kind of using the carbon point come the method for preparing silicon/carbon dioxide point composite, its technology
Scheme is：
Using sol-gal process：By the carbon dots solution containing full light carbon point of 0.1 described parts by volume, the positive silicic acid of 0.5 parts by volume
Ethyl ester is dissolved into the absolute ethyl alcohol of 20 parts by volume, and it is 2 that volume ratio is added after stirring:1 deionized water and ammoniacal liquor, is mixed
Solution, is transferred the solution into sampling box, is aged 10 hours, and deionized water and anhydrous second are removed within 8 hours in 100 DEG C of vacuum drying
Alcohol, obtains silicon/carbon dioxide point composite.
The present invention also provides a kind of method for preparing silicon/carbon dioxide point composite using the carbon point：
Using immersion deposition：0.1 ~ 1 gram of aperture 5-15nm nano SiO 2 particle is added to the ethanol of 3-5ml carbon point
In solution stir 30min after, be mixed thing in vacuum drying chamber 80 DEG C vacuum drying 15 hours after obtain nanometer titanium dioxide
Silicon/carbon point composite.
Advantages of the present invention is with effect：
The present invention is that can obtain carbon dots solution by a step solvent-thermal method, under portable 365 nanometers of ultra violet lamps, is synthesized
Carbon dots solution present red, orange, yellow, white, blue or green, blue, royal purple.The method of the full light carbon point of synthesis of the present invention is easy and effective, former
Material is cheap and easy to get, and reaction condition is gentle and environment-friendly, can be completed in common laboratory, it is easy to promote.
The present invention is described further with reference to specification drawings and specific embodiments.
Brief description of the drawings
Fig. 1：Pictorial diagram of the carbon point under uviol lamp（Red, orange, yellow, white, blue or green, blue, the royal purple carbon point of correspondence）；
Fig. 2：The UV absorption figure of carbon point（Red, orange, yellow, white, blue or green, blue, the royal purple carbon point of correspondence）；
Fig. 3：Red, orange, yellow, white, blue or green, blue, the royal purple carbon point of infrared spectrogram correspondence of carbon point）；
Fig. 4：(excitation wavelength is fluorescence spectra of the carbon dots solution in the case where different wavelengths of light is excited by 320nm to 540nm, step-length
20nm)。
Embodiment
The present invention is specifically described below by embodiment, is served only for that the present invention is further described, no
It is understood that for limiting the scope of the present invention, the technician in the field can be according to the content of foregoing invention to the present invention
Make some nonessential modifications and adaptations.
The present embodiment this method is initial reactant first with ammonium citrate and EDTA, in aqueous ammonia medium, using DMF as
Solvent, carbon dots solution is prepared by solvent thermal reaction.
Comprise the concrete steps that：Carbon source and passivator and ammoniacal liquor are put into solvent in the lump, reacted 3 ~ 8 hours at 80 ~ 110 DEG C
To synthesize full light carbon point；Passivator EDTA and the mass ratio of carbon source are 0.1 ~ 0.7, and the mass ratio of ammoniacal liquor and carbon source is 5 ~ 30, molten
The mass ratio of agent and carbon source is 25 ~ 100.Carbon source is ammonium citrate；Passivator is ethylenediamine tetra-acetic acid（EDTA）；Solvent is DMF
And deionized water.
Embodiment 1：
At room temperature, by 0.1 ~ 1.0 gram of lemon acid amide and 0.2 ~ 1.0 gram of EDTA, 2.5 grams of ammonia solvent to 100 grams of DMF
In, solution is transferred in hydrothermal reaction kettle, 100 ~ 200 DEG C are handled 3 ~ 8 hours, are naturally cooled to room temperature, are obtained claret
Carbon dots solution rubescent, orange, yellow, white, blue or green, blueness under uviol lamp；
As optional alternative, DMF can also use deionized water to replace, and can also realize blue or green, blue, royal purple carbon point.
Fig. 1 is full light carbon point prepared by the present embodiment 1, the pictorial diagram under ultraviolet light；Fig. 2 is prepared for the present embodiment
Carbon point UV absorption figure, it can be seen that the carbon point of preparation is mainly made up of surface groups such as hydroxyl, amino, carboxyls.
Fig. 3 is the infrared spectrogram of carbon point prepared by embodiment 1, and ~ 3420cm-1 is-OH absorption of vibrations ,~1640cm-
1 is C=O characteristic peak, and~1150cm-1 is the stretching vibration of P=O in the groups of-P=O (OH) 2.Infrared spectrum shows that ammoniacal liquor has been joined
With reacting and making carbon point surface-functionalized.
Fig. 4 is the fluorescence spectra of carbon dots solution made from the present embodiment.As seen from the figure, long wavelength's carbon point in full light carbon point
Peak position with excitation wavelength increase and keep constant, short wavelength's carbon point with excitation wavelength increase and there is Red Shift Phenomena.
Embodiment 2：
At room temperature, by 0.1 ~ 1.0 gram of lemon acid amide and 0.2 ~ 1.0 gram of EDTA, 2.5 grams of ammonia solvent to 100 grams go from
In sub- water, solution is transferred in hydrothermal reaction kettle, 100 ~ 200 DEG C are handled 3 ~ 8 hours, are naturally cooled to room temperature, are obtained wine red
The carbon dots solution of color rubescent, orange, yellow, white, blue or green, blueness under uviol lamp.
Embodiment 3：The preparation method of silicon/carbon dioxide point composite is prepared based on carbon quantum dot
Using sol-gal process：0.5ml tetraethyl orthosilicates are dissolved into 20ml absolute ethyl alcohols, after stirring add deionized water and
Ammoniacal liquor volume ratio is 2:1, mixed solution is obtained, is transferred the solution into sampling box, is aged 10 hours or so, it is true at 100 DEG C
Sky is dried 8 hours and removes deionized water and absolute ethyl alcohol.
Embodiment 4：The preparation method of silicon/carbon dioxide quantum dot composite material is prepared based on carbon quantum dot
Using immersion deposition：0.1 ~ 1 gram of aperture 5-15nm nano SiO 2 particle is added to the ethanol of 3-5ml carbon point
In solution stir 30min after, be mixed thing in vacuum drying chamber 80 DEG C vacuum drying 15 hours after obtain nanometer titanium dioxide
Silicon/carbon point composite.The mass fraction of carbon point is 20-35%g/ml in the ethanol solution of the carbon point.
Claims (3)
1. a kind of method for synthesizing full light carbon point, it is characterised in that comprise the following steps：
Carbon source and passivator and ammoniacal liquor are put into solvent in the lump, 3 ~ 8 hours are reacted at 80 ~ 110 DEG C to synthesize full light carbon point,
Obtain the carbon dots solution containing full light carbon point of claret, the mass ratio of passivator and carbon source is 0.1 ~ 0.7, ammoniacal liquor and carbon source
Mass ratio is 5 ~ 30, and the mass ratio of solvent and carbon source is 25 ~ 100, and carbon source is ammonium citrate；Passivator is ethylenediamine tetra-acetic acid；
Solvent is DMF or deionized water.
2. a kind of carbon point based on prepared by claim 1 methods described is come the method for preparing silicon/carbon dioxide point composite,
It is characterized in that：
Using sol-gal process：By the carbon dots solution containing full light carbon point of 0.1 described parts by volume, the positive silicic acid of 0.5 parts by volume
Ethyl ester is dissolved into the absolute ethyl alcohol of 20 parts by volume, and it is 2 that volume ratio is added after stirring:1 deionized water and ammoniacal liquor, is mixed
Solution, is transferred the solution into sampling box, is aged 10 hours, and deionized water and anhydrous second are removed within 8 hours in 100 DEG C of vacuum drying
Alcohol, obtains silicon/carbon dioxide point composite.
3. a kind of carbon point based on prepared by claim 1 methods described is come the method for preparing silicon/carbon dioxide point composite,
It is characterized in that：
Using immersion deposition：0.1 ~ 1 gram of aperture 5-15nm nano SiO 2 particle is added to the ethanol of 3-5ml carbon point
In solution stir 30min after, be mixed thing in vacuum drying chamber 80 DEG C vacuum drying 15 hours after obtain nanometer titanium dioxide
Silicon/carbon point composite.
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Cited By (7)
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| CN108998010A (en) * | 2018-07-04 | 2018-12-14 | 山西大学 | A kind of quick controllable preparation method of one step of full transmitting fluorescent carbon quantum dot |
| CN109266324A (en) * | 2018-10-16 | 2019-01-25 | 南京纳科伟业纳米技术有限公司 | Dendroid silica@carbon dots composite nanometer particle and preparation method thereof |
| WO2020045466A1 (en) * | 2018-08-31 | 2020-03-05 | 日産化学株式会社 | Method for producing photoluminescent nanocarbon |
| CN113735098A (en) * | 2020-05-29 | 2021-12-03 | 中国石油天然气股份有限公司 | Nitrogen-doped carbon nanoring, and preparation method and application thereof |
| CN113801657A (en) * | 2021-09-02 | 2021-12-17 | 西北工业大学 | Catecholamine specific response type iron-doped carbon nanodot and preparation method and application thereof |
| 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 |
| CN115466614A (en) * | 2022-09-26 | 2022-12-13 | 山东大学 | White luminescent soft material based on lanthanide series eutectic solvent and carbon dots and preparation method thereof |
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Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108998010A (en) * | 2018-07-04 | 2018-12-14 | 山西大学 | A kind of quick controllable preparation method of one step of full transmitting fluorescent carbon quantum dot |
| CN108998010B (en) * | 2018-07-04 | 2021-09-28 | 山西大学 | One-step rapid controllable preparation method of full-emission fluorescent carbon quantum dots |
| WO2020045466A1 (en) * | 2018-08-31 | 2020-03-05 | 日産化学株式会社 | Method for producing photoluminescent nanocarbon |
| CN109266324A (en) * | 2018-10-16 | 2019-01-25 | 南京纳科伟业纳米技术有限公司 | Dendroid silica@carbon dots composite nanometer particle and preparation method thereof |
| CN113735098A (en) * | 2020-05-29 | 2021-12-03 | 中国石油天然气股份有限公司 | Nitrogen-doped carbon nanoring, and preparation method and application thereof |
| CN113735098B (en) * | 2020-05-29 | 2023-08-22 | 中国石油天然气股份有限公司 | Nitrogen-doped carbon nano ring, and preparation method and application thereof |
| 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 |
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| CN113801657A (en) * | 2021-09-02 | 2021-12-17 | 西北工业大学 | Catecholamine specific response type iron-doped carbon nanodot and preparation method and application thereof |
| CN113801657B (en) * | 2021-09-02 | 2022-12-20 | 西北工业大学 | Catecholamine specific response type iron-doped carbon nanodot and preparation method and application thereof |
| CN115466614A (en) * | 2022-09-26 | 2022-12-13 | 山东大学 | White luminescent soft material based on lanthanide series eutectic solvent and carbon dots and preparation method thereof |
| CN115466614B (en) * | 2022-09-26 | 2024-04-05 | 山东大学 | White luminescent soft material based on lanthanide eutectic solvent and carbon dots and preparation method thereof |
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Application publication date: 20170915 |