CN102134485B - Method for mass production of water-soluble fluorescent carbon nanoparticles - Google Patents
Method for mass production of water-soluble fluorescent carbon nanoparticles Download PDFInfo
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Abstract
The invention discloses a method for mass production of water-soluble fluorescent carbon nanoparticles, which comprises the following steps: adding activated carbon, which is used as a carbon source, into an oxidant water solution, and stirring the mixed solution by a magnetic stirrer to obtain a black suspension; treating the suspension with ultrasonic in a 300W ultrasonic cleaning apparatus under the frequency of 40KHz for 2-4 hours; after the ultrasonic reaction finishes, carrying out vacuum filtration on the suspension to obtain a brownish black filtrate; and drying the filtrate by distillation at 60-70 DEG C, and dissolving the obtained black solid in deionized water at room temperature to obtain the purified water-soluble carbon nanoparticles. In the method disclosed by the invention, the water-soluble carbon nanoparticles, which can emit fluorescence from the visible light region to the near-infrared light region and has upconversion fluorescence property and other excellent optical properties, are synthesized under the action of the ultrasonic and strong oxidant. The method disclosed by the invention is simple and easy to implement, and has the advantages of low price, accessible raw materials and environmental protection.
Description
Technical field
The invention belongs to the preparation field of nano material, relate in particular to a kind of preparation method with carbon nano-particles of water-soluble and fluorescence property.
Background technology
Because be worth at electronics and the potential huge applications of biological field, fluorescent nano particles has caused the huge concern of recent scientific circles.At present, typical fluorescent particles be from lead, cadmium, silicon and the development of their compound and, but the people's that these materials have also caused for the potential hazard of environment aspect and weak light stability common concern.
The nanostructure of carbon is considered to the basic structural unit of following electron device, novel luminescent material and catalytic material, have great potential using value at bio-sensing and biomedical sector, correlative study is significant in nano science and technical field.Because the influence of quantum size effect and dielectric confinement effect, undersized carbon nano-particles have unique photoelectric property, make it demonstrate tempting application prospect in luminous, illumination and biomedical sector.In recent years, because the needs of basic science field and technology application facet, the carbon material of various forms type (as carbon nanotube, soccerballene, carbon nano rod, carbon nano-particles etc.) develops rapidly, fluorescent carbon nano-particles has huge potential using value at nano biological and catalytic field, than traditional quantum dot and organic dye, carbon nano-particles is at unreactiveness, stability, hypotoxicity and be easy to aspects such as modification and shown huge advantage.Therefore a kind of nanoparticle that has fluorescence property and can be applied in biological field should stablize, low toxicity and can send the fluorescence of character excellence.Yet, also exist many problems to need to solve at present in this area research, wherein comparatively outstanding is the method very complicated comparatively of carbon nano-particles preparation, and it is single to have photoluminescent property simultaneously, is difficult to shortcomings such as purification.For the ease of the further application of carbon-based nano device preparation and carbon nano-structured material, it is very necessary and significant developing a kind of carbon nano-particles preparation method simple and that have an excellent photoluminescent property.
In the nanostructure of carbon, for example the synthetic aspect of carbon nano-particles has the report about multiple preparation method, for example: laser lift-off graphite (typical bibliographical information: Sun, Y.P.; Zhou, B.; Lin, Y.; Wang, W.; Fernando, K.A.S.; Pathak, P.; Meziani, M.J.; Harruff, B.A.; Wang, X.; Wang, H.; Luo, P.G.; Yang, H.; Kose, M.E.; Chen, B.; Veca, L.M.; Xie, S.Y.J.Am.Chem.Soc.2006,128,7756; Cao, L.; Wang, X.; Meziani, M.J.; Lu, F.; Wang, H.; Luo, P.G.; Lin, Y.; Harruff, B.A.; Veca, L.M.; Murray, D.; Xie, S.Y.; Sun, Y.P.J.Am.Chem.Soc.2007,129,11318; Hu, S.L.; Niu, K.Y.; Sun, J.; Yang, J.; Zhao, N.Q.; Du, X.W.J.Mater.Chem.2009,19,484; Wang, X.; Cao, L.; Lu, F.S.; Meziani, M.J.; Li, H.; Qi, G.; Zhou, B.; Harruff, B.A.; Kermarrec, F.; Sun, Y.P.Chem.Commun.2009,3774.), electrochemical oxidation graphite (typical bibliographical information: Zhao, Q.L.; Zhang, Z.L.; Huang, B.H.; Peng, J.; Zhang, M.; Pang, D.W.Chem.Commun.2008,5116; Zheng, L.Y.; Chi, Y.W.; Dong, Y.Q.; Lin, J.P.; Wang, B.B.J.Am.Chem.Soc.2009,131,4564.), electrochemistry soaks into carbon nanotube (typical bibliographical information: Xu, X.; Ray, R.; Gu, Y.; Ploehn, H.J.; Gearheart, L.; Raker, K.; Scrivens, W.J.Am.Chem.Soc.2004,126,12736; Bottini, M.; Balasubramanian, C.; Dawson, M.I.; Bergamaschi, A.; Bellucci, S.; Mustelin, T.J.Phys.Chem.B 2006,110, and 831; Zhou, J.; Booker, C.; Li, R.; Zhou, X.; Sham, T.K.; Sun X.; Ding, Z.J.Am.Chem.Soc.2007,129,744.), the relevant precursor of hydro-thermal (typical bibliographical information: Sun, X.M.; Li, Y.D.Angew.Chem.Int.Ed.2004,43,597; Bourlinos, A.B.; Stassinopoulos, A.; Anglos, D.; Zboril, R.; Georgakilas, V.; Giannelis, E.P.Chem.Mater.2008,20,4539; Bourlinos, A.B.; Stassinopoulos, A.; Anglos, D.; Zboril, R.; Karakassides, M.; Giannelis, E.P.Small 2008,4,455.), arc-over (typical bibliographical information: Liu, H.P.; Ye, T.; Mao, C.D.Angew.Chem.2007,119,6593; Angew.Chem.Int.Ed.2007,46,6473; Tian, L.; Ghosh, D.; Chen, W.; Pradhan, S.; Chang, X.; Chen, S.W.Chem.Mater.2009,21,2803; Ray, S.C.; Saha, A.; Jana, N.R.; Sarkar, R.J.Phys.Chem.B.2009,113,18546.), Nano diamond peel off (typical bibliographical information: Yu, S.J.; Kang, M.W.; Chang, H.C.; Chen, K.M.; Yu, Y.C.J.Am.Chem.Soc.2005,127,17604; Fu, C.C.; Lee, H.Y.; Chen, K.; Lim, T.S.; Wu, H.Y.; Lin, P.K.; Wei, P.K.; Tsao, P.H.; Chang, H.C.; Fann, W.; Proc.Natl.Acad.Sci.U.S.A.2007,104,727.), microwave is synthetic and wet-chemical synthetic (typical bibliographical information: Zhu, H.; Wang, X.L.; Li, Y.L.; Wang, Z.J.; Yang, F.; Yang, X.R.Chem.Commun.2009,5118; Liu, R.L; Wu, D.Q.; Liu, S.H.; Koynov, K.; Knoll, W.; Li, Q.Angew.Chem.Int.Ed.2009,48,4598.) etc.
But these preparation methods can't realize carbon nano-structured simple synthesizing at present, and the process that aftertreatment is purified is more complicated also, and the photoluminescent property of resulting carbon nano-particles is also more single.For the easy manufacture that realizes carbon nano-particles and the carbon nano-particles that obtains having excellent fluorescence property, develop a kind of carbon nano-particles preparation method with these photoluminescent properties and be very important.These photoluminescent properties comprise emission from visible region to near-infrared region fluorescence and the fluorescence with last conversion character, applied research is significant these photoluminescent properties to biological field, yet yet there are no report about a large amount of, the easy synthetic method of the carbon nano-particles that has these two kinds of photoluminescent properties simultaneously.
Summary of the invention
Defective in view of above-mentioned prior art exists the objective of the invention is to propose the method that a kind of a large amount of preparation has the water-soluble carbon nanoparticle of excellent fluorescence property.This method is by the water-soluble carbon nanoparticle of ultrasonic wave and strong oxidizer effect preparation, have emission from visible region to near-infrared region fluorescence and the excellent optical such as fluorescence with last conversion character, simple, cheap, starting material are easy to get, environmental protection.
Purpose of the present invention will be achieved by the following technical programs:
A kind of a large amount of method for preparing water-soluble fluorescent carbon nano-particles may further comprise the steps:
Step 1: be carbon source with the gac, get 2～4g gac and join in 70～200ml aqueous oxidizing agent solution, the reaction vessel that the two mixed solution is housed is placed on stirs 10～15 minutes on the magnetic stirring apparatus, make the suspension of black after stirring;
Step 2: the reaction vessel in the step 1 is put in the 300W power ultrasonic cleaning apparatus under frequency 40KHz ultrasonic 2～4 hours;
Step 3: after ultrasonic reaction finishes, the suspension vacuum filtration is handled, obtained the filtrate of brownish black;
Step 4: the filtrate that step 3 is obtained at room temperature is dissolved in the black solid that obtains in the deionized water at 60～70 ℃ of following evaporates to dryness, obtains the water-soluble carbon nanoparticle behind the purifying.
Further, above-mentioned a kind of a large amount of methods that prepare water-soluble fluorescent carbon nano-particles, wherein: the oxygenant in the described step 1 is strong oxidizer.
Further, above-mentioned a kind of a large amount of methods that prepare water-soluble fluorescent carbon nano-particles, wherein: the oxygenant in the described step 1 comprises hydrogen peroxide.
Further, above-mentioned a kind of a large amount of methods that prepare water-soluble fluorescent carbon nano-particles, wherein: the oxygenant in the described step 1 is hydrogen peroxide, hydrogen peroxide quality percentage composition or volumn concentration are 20%～40% in the hydrogen peroxide solution.
Further, above-mentioned a kind of a large amount of methods that prepare water-soluble fluorescent carbon nano-particles, wherein: the reaction vessel in the described step 1 is glass material.
Further, above-mentioned a kind of a large amount of methods that prepare water-soluble fluorescent carbon nano-particles, wherein: the reaction vessel relative response thing in the described step 1 is the material of inertia, comprises the Teflon.
Further, above-mentioned a kind of a large amount of methods that prepare water-soluble fluorescent carbon nano-particles, wherein: the filter paper that the vacuum filtration in the described step 3 is used is 300 order middling speed filter paper.
Further, above-mentioned a kind of a large amount of methods that prepare water-soluble fluorescent carbon nano-particles, wherein: the gac in the described step 1 and the purity of oxygenant all are analytical pure, and the solvent of aqueous oxidizing agent solution is deionized water.
Method of the present invention is to utilize the strong oxidizing property of oxygenant and hyperacoustic swing crushing function to assist the synthesize nano carbon particle.After reaction finishes, the carbon nano-particles that obtains:
1) has well water-soluble, can dissolve each other arbitrarily with water;
2) particle diameter can be dispersed in the reaction soln uniformly at 5～12nm, and the surface has abundant oxy radical (hydroxyl, carboxyl etc.), and is surface-functionalized or nanoparticle modified than being easier to;
3) photoluminescent property excellence has the photoluminescent property that good UV, visible light excites visible emissivity, and its emmission spectrum can change along with the change of excitation wavelength; Have abundant up-conversion fluorescence character, its emmission spectrum can change along with the change of excitation wavelength, and up-conversion fluorescence has and low-energy light can be converted to high-octane light, and the radiative intensity difference that obtains under different excitation wavelengths.
Description of drawings
Fig. 1 a is transmission electron microscope (TEM) photo of the carbon nano-particles for preparing among the inventive method embodiment 1;
Fig. 1 b is the in kind photo of the carbon nano-particles aqueous solution under natural light irradiation for preparing among the inventive method embodiment 1;
Fig. 1 c is the in kind photo of the carbon nano-particles aqueous solution under UV-light (365nm) irradiation for preparing among the inventive method embodiment 1
Fig. 1 d is the photoluminescence spectra (vignette be 700 enlarged views to 1000nm place) of carbon nano-particles under the 350nm irradiation for preparing among the inventive method embodiment 1;
Fig. 1 e is the x X-ray photoelectron spectroscopy X figure of the carbon nano-particles for preparing among the inventive method embodiment 1;
Fig. 2 is the histogram of particle size distribution of the carbon nano-particles for preparing among the inventive method embodiment 1;
Fig. 3 a～Fig. 3 d is the fluorescence pictorial diagram of carbon nano-particles solid under the different wave length exciting light for preparing among the inventive method embodiment 1;
Fig. 3 e is the fluorescence spectrum figure of carbon nano-particles under UV-light and excited by visible light for preparing among the inventive method embodiment 1;
Fig. 4 a is the up-conversion fluorescence spectrogram of the carbon nano-particles for preparing among the inventive method embodiment 1;
Fig. 4 b is the ultraviolet spectrogram of the carbon nano-particles for preparing among the inventive method embodiment 1.
Embodiment
The present invention adopts ultrasonic synthetic method, by the assistance of oxidants hydrogen peroxide, realizes simply preparing in large quantities the abundant water-soluble carbon nanoparticle (diameter 5～12 nanometers) of photoluminescent property.
Below by specific embodiment method of the present invention is described, but the present invention is not limited thereto.Experimental technique described in the following embodiment if no special instructions, is ordinary method; Described reagent and material if no special instructions, all can obtain from commercial channels.
Embodiment 1
It is preparation carbon nano-particles carbon source with the gac, getting 2～4g gac, to join 70～200ml hydrogen peroxide quality percentage composition (or volumn concentration) be in 30% the hydrogen peroxide solution, the glass reaction container (or other materials such as Teflon) that the two mixed solution is housed is placed on the magnetic stirring apparatus stirred 10 minutes, make the suspension of black after stirring, then reaction vessel is put in the 300W power ultrasonic cleaning apparatus, under frequency 40KHz ultrasonic 2～4 hours, after reaction finishes the suspension vacuum filtration is handled (suction filtration filter paper is 300 order middling speed filter paper), obtain the filtrate of brownish black, at last with filtrate 60 ℃ slowly evaporate to dryness remove unreacted hydrogen peroxide, the black solid that obtains at room temperature is dissolved in the deionized water, obtains the water-soluble carbon nanoparticle behind the purifying.The gac that aforesaid method is used and the purity of hydrogen peroxide all are analytical pure, and the solvent of hydrogen peroxide solution is deionized water.
Fig. 1 a is transmission electron microscope (TEM) photo of the carbon nano-particles for preparing in the present embodiment 1; Fig. 1 b and Fig. 1 c are respectively the in kind photo of the above-mentioned carbon nano-particles aqueous solution under natural light and UV-light (365nm) irradiation, and wherein the color of solution is light yellow among Fig. 1 b, and the color of solution is blue among Fig. 1 c; Fig. 1 d be above-mentioned carbon nano-particles under 350nm irradiation photoluminescence spectra of (vignette is 700 enlarged views to the 1000nm place), emmission spectrum covers UV, visible light to near-infrared region, illustrates that carbon nano-particles has the photoluminescent property that good UV, visible light excites visible emissivity; Fig. 1 e is the x X-ray photoelectron spectroscopy X figure of above-mentioned carbon nano-particles, and carbon nano-particles mainly is made up of carbon and oxygen element as we can see from the figure.
This histogram of particle size distribution for the carbon nano-particles for preparing among the embodiment 1 of Fig. 2 can find out that the particle diameter of carbon nano-particles mainly is distributed in 5～12nm.
Fig. 3 a～Fig. 3 d is the fluorescence pictorial diagram of carbon nano-particles solid under the different wave length exciting light for preparing in the present embodiment 1, and excitation wavelength is respectively 360nm, and 390nm, 470nm and 540nm, fluorescence color are followed successively by blueness, green, yellow and red.Fig. 3 e is that above-mentioned carbon nano-particles is under UV-light and excited by visible light, (excitation wavelength is 300nm to the fluorescence spectrum figure of carbon nano-particles emission, 350nm, 400nm, 450nm, 500nm, 550nm and 600nm), wherein to represent excitation wavelength respectively be 300nm to curve A～G, 350nm, 400nm, 450nm, 500nm, the fluorescence spectrum figure when 550nm and 600nm, illustrate that carbon nano-particles has the photoluminescent property that good UV, visible light excites visible emissivity, its emmission spectrum can change along with the change of excitation wavelength.
Fig. 4 a prepares the up-conversion fluorescence spectrogram of carbon nano-particles (excitation wavelength is respectively 600nm in the present embodiment, 650nm, 700nm, 750nm, 800nm, 850nm, 900nm, 950nm and 1000nm), wherein to represent excitation wavelength respectively be 600nm to curve 1～9,650nm, 700nm, 750nm, 800nm, 850nm, 900nm, the fluorescence spectrum figure when 950nm and 1000nm illustrates that carbon nano-particles has abundant up-conversion fluorescence character, its emmission spectrum can change along with the change of excitation wavelength, and up-conversion fluorescence has and low-energy light can be converted to high-octane light.Fig. 4 b is the ultraviolet spectrogram of above-mentioned carbon nano-particles, the ultraviolet spectrogram of gained, and its peak position is similar to the uv-absorbing of typical aromatic hydrocarbon substance at 200～300nm.
It is preparation carbon nano-particles carbon source with the gac, getting the 3g gac, to join 100ml hydrogen peroxide quality percentage composition (or volumn concentration) be in 40% the hydrogen peroxide solution, to glass reaction container (or other material reaction vessels of the two mixed solution be housed, as Teflon) be placed on the magnetic stirring apparatus and stirred 15 minutes, make the suspension of black after stirring, then reaction vessel is put in the 300W power ultrasonic cleaning apparatus, under frequency 40KHz ultrasonic 3.5 hours, after reaction finishes the suspension vacuum filtration is handled (suction filtration filter paper is 300 order middling speed filter paper), obtain the filtrate of brownish black, at last with filtrate 70 ℃ slowly evaporate to dryness remove unreacted hydrogen peroxide, the black solid that obtains at room temperature is dissolved in the deionized water, obtains the water-soluble carbon nanoparticle behind the purifying.The gac that aforesaid method is used and the purity of hydrogen peroxide all are analytical pure, and the solvent of hydrogen peroxide solution is deionized water.The quality percentage composition (or volumn concentration) of hydrogen peroxide is in 20%～40% scope, can both reach good oxidation effectiveness, wherein when the quality percentage composition (or volumn concentration) of hydrogen peroxide is 40%, can provide more oxygenant for reaction, discharge the oxygen bubble of maximum in the ultrasonic procedure, can in reaction process, contact more closely with gac, make faster and better the finishing of reaction.
Claims (2)
1. method for preparing in a large number water-soluble fluorescent carbon nano-particles may further comprise the steps:
Step 1: be carbon source with the gac, getting 2 ~ 4g gac, to join 70 ~ 200ml quality percentage composition or volumn concentration be in 20% ~ 40% the aqueous hydrogen peroxide solution, the reaction vessel that the two mixed solution is housed is placed on stirs 10 ~ 15 minutes on the magnetic stirring apparatus, make the suspension of black after stirring;
Step 2: the reaction vessel in the step 1 is put in the 300W power ultrasonic cleaning apparatus under frequency 40KHz ultrasonic 2 ~ 4 hours;
Step 3: after ultrasonic reaction finishes, the suspension vacuum filtration is handled, obtained the filtrate of brownish black, the used filter paper of described vacuum filtration is 300 order middling speed filter paper;
Step 4: the filtrate that step 3 is obtained at room temperature is dissolved in the black solid that obtains in the deionized water at 60 ~ 70 ℃ of following evaporates to dryness, obtains particle diameter behind the purifying at the water-soluble carbon nanoparticle of 5nm ~ 12nm;
Reaction vessel in the described step 1 is glass material or Teflon.
2. a kind of a large amount of methods that prepare water-soluble fluorescent carbon nano-particles according to claim 1, it is characterized in that: the gac in the described step 1 and the purity of hydrogen peroxide all are analytical pure, and the solvent of aqueous hydrogen peroxide solution is deionized water.
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| CN102604629A (en) * | 2012-02-08 | 2012-07-25 | 中国人民解放军军事医学科学院卫生装备研究所 | Preparation method and applications of amino carbon quantum dots |
| JP6085880B2 (en) * | 2013-01-11 | 2017-03-01 | 国立研究開発法人産業技術総合研究所 | Carbon quantum dot manufacturing method and carbon quantum dot |
| CN103086356A (en) * | 2013-02-19 | 2013-05-08 | 复旦大学 | Method for preparing carbon quantum dots |
| CN104117375B (en) * | 2014-06-18 | 2017-01-11 | 南京大学 | Preparation method of synthesized carbon quantum dot-carbon nitrogen macromolecule composite infrared light catalyst |
| CN106566541A (en) * | 2016-10-25 | 2017-04-19 | 大连理工大学 | Environmentally-friendly method for preparing fluorescent carbon quantum dots with activated carbon |
| CN109337680B (en) * | 2018-11-07 | 2022-04-19 | 广州大学 | Preparation method of BCNO quantum dots |
| CN110187124B (en) * | 2019-05-20 | 2022-10-04 | 上海凯创生物技术有限公司 | Preparation method and application of carbon quantum dots |
| CN114455567B (en) * | 2020-11-03 | 2023-06-30 | 广东量子墨滴生物科技有限公司 | Preparation method and application of carbon nano particles |
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| CN1884430A (en) * | 2006-06-30 | 2006-12-27 | 上海师范大学 | Fluorescent carbon nanometer tube and its preparation method and application |
| CN101186763A (en) * | 2007-11-08 | 2008-05-28 | 上海交通大学 | Method for preparing fluorescence ion liquid functionalization carbon nano-tube |
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| CN101186763A (en) * | 2007-11-08 | 2008-05-28 | 上海交通大学 | Method for preparing fluorescence ion liquid functionalization carbon nano-tube |
| CN101787278A (en) * | 2010-03-17 | 2010-07-28 | 上海大学 | Pyrolytic synthesis method for water-soluble fluorescent carbon nano-particles |
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