CN102849722A - Carbon nano-dot, and preparation method and application thereof - Google Patents
Carbon nano-dot, and preparation method and application thereof Download PDFInfo
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- CN102849722A CN102849722A CN2012103128440A CN201210312844A CN102849722A CN 102849722 A CN102849722 A CN 102849722A CN 2012103128440 A CN2012103128440 A CN 2012103128440A CN 201210312844 A CN201210312844 A CN 201210312844A CN 102849722 A CN102849722 A CN 102849722A
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Abstract
The invention discloses a carbon nano-dot, and a preparation method and an application thereof, and solves a problem that the application of present nano-dots is restricted because of high preparation cost and easy fluorescent quenching appearance of an aggregate state. According to the invention, the carbon nano-dot having a high fluorescence quantum efficiency is prepared through adopting a polycarboxyl or polyhydroxy contained organic compound, or an amino acid as a raw material, and urea as a surface passivation modification agent, and through a microwave process, and a carbon nano-dot fluorescent ink is prepared through using the carbon nano-dot. The preparation method disclosed in the invention has the advantages of simplicity, low cost and convenient large-scale production; the fluorescent quenching of the prepared carbon nano-dot on the surface of a biological product does not appear, and the highest fluorescence quantum efficiency is 42%; and the prepared carbon nano-dot fluorescent ink is nontoxic, does not generate a precipitate after long-time dispose, and can be applied to the biological imaging field, the biological product identification field, the information storage field, the information encryption field, the false proof field, the illumination display field, the photovoltaic device field and the like.
Description
Technical field
The present invention relates to a kind of carbon nano dot and preparation method thereof and application, belong to the nanometer material science field.
Background technology
The carbon nano dot is a kind of novel nano material, because its advantage with many uniquenesses is (such as chemical stability, without optical flare, fast lightly float, nontoxic, excellent biocompatibility) and be subject to increasing concern (Luminescent Carbon Nanodots:Emergent Nanolights, Sheila N. Baker, Gary A. Baker, Angew. Chem. Int. Ed., 2010,49,6726).Carbon nano dot with fluorescent characteristic has potential application in fields such as bio-imaging, laser, photoelectric devices.
The carbon nano dot can be prepared by several different methods, such as laser ablation, electrochemical process, arc discharge method, pyrolysis method, excusing from death and microwave method.In these methods, microwave method is low owing to cost, relative environmental protection is had an high regard for.Microwave method can improve rapidly the temperature of reactant, and fast reaction speed and pyrolysis rate can be realized the pyrolysis legal effect and significantly shorten preparation time.Pyrolysis method and microwave method prepare the carbon nano dot usually to contain many carboxyls or polyhydric organic compound as starting material, for example, document (Microwave synthesis of fluorescent carbon nanoparticles with electrochemiluminescence properties, Hui Zhu, Xiaolei Wang, Yali Li, Zhongjun Wang, Fan Yang, Xiurong Yang, Chem. Commun., 2009,51), take carbohydrate derivatives such as glucose and fructose as raw material, prepare the carbon nano dot by microwave method; Document (Microwave assisted one-step green synthesis of cell-permeable multicolor photoluminescent carbon dots without surface passivation reagents, Xiaohui Wang, Konggang Qu, Bailu Xu, Jinsong Ren, Xiaogang Qu, J. Mater. Chem., 2011,21,244), take glycerine as raw material, prepare the carbon nano dot by microwave method; Document (Tuning of photoluminescence on different surface functionalized carbon quantum dots, Sourov Chandra, Shaheen H. Pathan, Shouvik Mitra, Binita H. Modha, Arunava Goswami, Panchanan Pramanik, RSC Adv., 2012,2,3602), take chitosan, Lalgine and starch as raw material, prepare the carbon nano dot by microwave method.
In order to obtain to have the carbon nano dot of fluorescent characteristic, usually need to introduce the surface passivation modifier that contains polymer chain.For example, document (Microwave synthesis of fluorescent carbon nanoparticles with electrochemiluminescence properties, Hui Zhu, Xiaolei Wang, Yali Li, Zhongjun Wang, Fan Yang, Xiurong Yang, Chem. Commun., 2009,51), take carbohydrate derivatives such as glucose and fructose as raw material, in the situation without the surface passivation modifier, the carbon nano dot for preparing by microwave method shows very weak fluorescence, after adding polyoxyethylene glycol (molecular-weight average 200) is as the surface passivation modifier, carbon nano dot by the microwave method preparation shows the fluorescent appear of enhancing, fluorescence quantum efficiency 3%-6%.But the cost of surface passivation modifier that contains polymer chain is higher, and the residual surface passivation modifier that contains polymer chain is difficult for removing.The carbon nano dot can have good dispersing characteristic at the dilute solution state, and the dilute solution of the carbon nano dot of surface passivation can show than strong fluorescent properties.And under state of aggregation, the material nano dimensional effect disappears, and can show strong fluorescent quenching phenomenon, has greatly limited the application of such material in the solid luminescent system.Do not have simultaneously also in the prior art that preparation cost is low, the preparation method is simple, environmental protection, show high-fluorescence quantum yield in the solid-state system, and can be applied to carbon nano dot in the daily life.
Summary of the invention
The object of the invention is to reduce the preparation cost of fluorescent carbon nano dot, widen the Application Areas of carbon nano dot, a kind of carbon nano dot and preparation method thereof and application are provided.
The invention provides a kind of carbon nano dot, this carbon nano dot is to contain many carboxyls or polyhydric organic compound is raw material, or take amino acid as raw material, is prepared from take urea as the surface passivation agent, and step is as follows:
1. urea with contain many carboxyls or polyhydric organic compound, or amino acid in mass ratio 0.1:1-4:1 be mixed with the aqueous solution;
2. the 1. prepared aqueous solution is obtained the brownish black solid by the microwave heating reaction;
3. with the brownish black solid through heating under vacuum, remove residual micromolecular compound, namely obtain the carbon nano dot.
Preferably, described many carboxyls or polyhydric organic compound are citric acid, ethylenediamine tetraacetic acid (EDTA), glycerine, glucose, fructose, sucrose, chitosan or starch; More preferably, citric acid, glycerine, glucose or sucrose; Citric acid most preferably.
Preferably, described amino acid is glycine or L-glutamic acid; More preferably, glycine.
Preferably, step 1. in, described urea with contain many carboxyls or polyhydric organic compound, or amino acid in mass ratio 0.1:1-4:1 be mixed with saturated aqueous solution.
Preferably, step 2. in, the described aqueous solution is through 500-900W power microwave heating 3-10 minute, more preferably through 700W power microwave heating 4 minutes.
Preferably, step 3. in, the vacuum tightness of described heating under vacuum is the 0.001-0.1 handkerchief, Heating temperature is 50-70 degree centigrade, 1-2 hour heat-up time; More preferably, the vacuum tightness of described heating under vacuum is 0.01 handkerchief, and Heating temperature is 60 degrees centigrade, 1 hour heat-up time.
The invention provides a kind of preparation method of carbon nano dot, may further comprise the steps:
1. urea with contain many carboxyls or polyhydric organic compound, or amino acid 0.1:1-4:1 obtained aqueous solution in mass ratio;
2. the 1. prepared aqueous solution is obtained the brownish black solid by the microwave heating reaction;
3. with the brownish black solid through heating under vacuum, remove residual micromolecular compound, obtain the carbon nano dot.
The present invention also provides the application of a kind of carbon nano dot in the preparation fluorescent ink, is that the carbon nano dot is soluble in water, through centrifugal, obtains supernatant liquor; The supernatant liquor that obtains through water or organic solvent diluting, is obtained carbon nano dot fluorescent ink.
Preferably, described organic solvent is ethanol.
Preferably, centrifugal rotational speed is 2000-4000 rev/min, and the time is 15-30 minute; More preferably, centrifugal rotational speed is 3000 rev/mins, and the time is 20 minutes.
Beneficial effect of the present invention:
(1) the present invention is to contain many carboxyls or polyhydric organic compound, or amino acid is raw material, with urea as the surface passivation modifier, the carbon nano dot for preparing high fluorescence quantum efficiency by microwave method, overcome prior art with polymer chain as surface passivation modifier preparation cost is high, quenching of fluorescence easily occurs state of aggregation problem, preparation method of the present invention is simple, and cost is low, is convenient to scale operation;
(2) the prepared carbon nano dot maximum fluorescence quantum yield of the present invention can be up to being 42%;
(3) abundant amide group and carboxyl are contained in the prepared carbon nano dot surface of the present invention, has excellent biocompatibility, can effectively disperse to be attached to the solid-state biological product such as paper, vegetable fibre, fur surface, avoid the carbon nano dot to reunite, keep the strong fluorescence emitting characteristics of carbon nano dot, its fluorescence emission peak depends on excitation wavelength; The carbon nano dot of preparation is attached to inorganic materials, plastics, man-made fiber surface, and the carbon nano dot is reunited, and its fluorescent emission Da Fu temper goes out, and according to this characteristic, carbon nano dot of the present invention can be used as the appraisal basis of biological product;
(4) the prepared carbon nano dot fluorescent ink of the present invention is nontoxic, permanent placement can not produce precipitation, has strong fluorescent characteristic, mark fluorescent graphic on skin safely may be used on the multiple fields such as bio-imaging, biological product evaluation, information storage, information encryption, false proof, illumination demonstration, photovoltaic device.
Description of drawings
Fig. 1 is the transmission electron microscope picture of the carbon nano dot of the embodiment of the invention 1;
Fig. 2 be in the atomic power scanned picture of carbon nano dot of the embodiment of the invention 1 and the atomic power scanned picture A to the altitude curve of B position;
Fig. 3 is the infrared spectrogram of the carbon nano dot of the embodiment of the invention 1;
Fig. 4 is the ultra-violet absorption spectrum and fluorescence emission spectrogram under different excitation wavelengths of the aqueous solution of the carbon nano dot of the embodiment of the invention 12;
Fig. 5 is that the carbon nano dot fluorescent ink of the embodiment of the invention 12 drips on the filter paper, behind the air drying, and the fluorescence emission spectral curve under different excitation wavelengths;
Fig. 6 is that the carbon nano dot fluorescent ink of the embodiment of the invention 12 makes growth of mung beans become to have the photo under different-waveband illumination of the bean sprouts of fluorescent characteristic;
Fig. 7 is the fluorescence spectrum figure of the urine of carbon nano dot fluorescent ink in the time of one month under different excitation wavelengths that big white mouse is drunk the embodiment of the invention 12;
Fig. 8 is the carbon nano dot fluorescent ink after month that big white mouse is drunk the embodiment of the invention 12, stops to drink carbon nano dot fluorescent ink, changes and drinks the fluorescence spectrum figure of the urine of normal tap water in the time of 1 month under different excitation wavelengths;
Fig. 9 is the fluorescence spectrum figure of urine under different excitation wavelengths that big white mouse is drunk normal tap water;
Figure 10 is the carbon nano dot fluorescent ink of the embodiment of the invention 12 and is purchased the green fluorescence pen consists of enciphered digital at paper fluorescence photo;
Figure 11 is the cotton thread and the photo of nylon fiber under different excitation wavelengths of being infected with the carbon nano dot fluorescent ink of not being infected with the embodiment of the invention 12;
Figure 12 for the carbon nano dot fluorescent ink that uses the embodiment of the invention 12 at the photo of fingerprint trace under different excitation wavelengths that paper stays;
Figure 13 is the carbon nano dot fluorescent ink of the embodiment of the invention 12 stays fluorescent graphic at skin fluorescence photo;
Figure 14 is the fluorescence emission spectrogram of ethanolic soln under different excitation wavelengths of the carbon nano dot of the embodiment of the invention 13;
Figure 15 is the fluorescence emission spectrogram of the aqueous solution under different excitation wavelengths of the carbon nano dot of the embodiment of the invention 14;
Figure 16 is that the carbon nano dot fluorescent ink of the embodiment of the invention 14 drips on the filter paper, after the dry air, and the fluorescence emission spectral curve under different excitation wavelengths;
Figure 17 is the fluorescence emission spectrogram of ethanolic soln under different excitation wavelengths of the carbon nano dot of the embodiment of the invention 15;
Figure 18 is the fluorescence emission spectrogram of the aqueous solution under different excitation wavelengths of the carbon nano dot of the embodiment of the invention 16;
Figure 19 is the fluorescence emission spectrogram of the aqueous solution under different excitation wavelengths of the carbon nano dot of the embodiment of the invention 17;
Figure 20 is that the carbon nano dot fluorescent ink of the embodiment of the invention 17 drips on the filter paper, behind the air drying, and the fluorescence emission spectral curve under different excitation wavelengths;
Figure 21 is the fluorescence emission spectrogram of ethanolic soln under different excitation wavelengths of the carbon nano dot of the embodiment of the invention 18;
Figure 22 is the fluorescence emission spectrogram of the aqueous solution under different excitation wavelengths of the carbon nano dot of the embodiment of the invention 19;
Figure 23 is the fluorescence emission spectrogram of the aqueous solution under different excitation wavelengths of the carbon nano dot of the embodiment of the invention 20;
Figure 24 is the fluorescence emission spectrogram of the aqueous solution under different excitation wavelengths of the carbon nano dot of the embodiment of the invention 21;
Figure 25 is the fluorescence emission spectrogram of the aqueous solution under different excitation wavelengths of the carbon nano dot of the embodiment of the invention 22.
Embodiment
The invention provides a kind of carbon nano dot, this carbon nano dot is to contain many carboxyls or polyhydric organic compound is raw material, or take amino acid as raw material, is prepared from take urea as the surface passivation agent, and step is as follows:
1. urea with contain many carboxyls or polyhydric organic compound, or amino acid 0.1:1-4:1 obtained aqueous solution in mass ratio;
2. the 1. prepared aqueous solution is obtained the brownish black solid by the microwave heating reaction;
3. the brownish black solid of preparation is removed residual micromolecular compound through heating under vacuum, obtains the carbon nano dot.
The performance of the carbon nano dot of the present invention's preparation depends on the raw material of preparation carbon nano dot and the mass ratio of selected raw material and urea and concerns; When urea with contain many carboxyls or polyhydric organic compound, or amino acid in mass ratio 0.1:1-4:1 be mixed with saturated aqueous solution, the performance of the carbon nano dot of preparation is better; As long as contain many carboxyls or polyhydric organic compound, or amino acid all can be used as raw material of the present invention and prepares the carbon nano dot; Urea is purchased and gets final product without limits.
Preferably, describedly contain many carboxyls or polyhydric organic compound is citric acid, ethylenediamine tetraacetic acid (EDTA), glycerine, glucose, fructose, sucrose, chitosan or starch; More preferably, citric acid, glycerine, glucose or sucrose; Citric acid most preferably.
Preferably, described amino acid is glycine or L-glutamic acid; More preferably, glycine.
The microwave heating of step of the present invention in 2. is technology well known in the art, preferably, the aqueous solution is 1. put into microwave oven, through 500-900W power microwave heating 3-10 minute; More preferably through 700W power microwave heating 4 minutes.
Preferably, step 3. in, the vacuum tightness of described heating under vacuum is the 0.001-0.1 handkerchief, Heating temperature is 50-70 degree centigrade, 1-2 hour heat-up time; More preferably, the vacuum tightness of described heating under vacuum is 0.01 handkerchief, and Heating temperature is 60 degrees centigrade, 1 hour heat-up time.
The micromolecular compound that 3. step of the present invention removes mainly is residual urea.
The invention provides a kind of preparation method of carbon nano dot, may further comprise the steps:
1. urea with contain many carboxyls or polyhydric organic compound, or amino acid in mass ratio 0.1:1-4:1 be mixed with the aqueous solution;
2. the 1. prepared aqueous solution is obtained the brownish black solid by the microwave heating reaction;
3. prepare the brownish black solid through heating under vacuum, remove residual micromolecular compound, obtain the carbon nano dot.
The present invention also provides the application of a kind of carbon nano dot in the preparation fluorescent ink, is in the carbon nano dot is water-soluble or the organic solvent, through centrifugal, obtains supernatant liquor; The supernatant liquor that obtains through water or organic solvent diluting, is obtained carbon nano dot fluorescent ink.
Preferably, described organic solvent is ethanol.
Preferably, centrifugal rotational speed is 2000-4000 rev/min, and the time is 15-30 minute; More preferably, centrifugal rotational speed is 3000 rev/mins, and the time is 20 minutes.
Further specify the present invention below in conjunction with embodiment, it is commercially available to use material to pass through among the embodiment.
Embodiment 1-11 is the Preparation Example of carbon nano dot of the present invention.
In conjunction with Fig. 1-3 explanation embodiment 1
The preparation of carbon nano dot of the present invention:
1. 3 gram urea and 3 gram citric acids are dissolved in 10 ml waters;
2. 1. prepared urea and lemon aqueous acid are placed in the microwave oven, through 700W power microwave heating 4 minutes, obtain the brownish black solid;
3. the brownish black solid with preparation is placed in the vacuum drying oven, and vacuum tightness is 0.01 handkerchief, and temperature is 60 degrees centigrade, heats 1 hour, removes residual micromolecular compound, obtains the carbon nano dot.
Fig. 1 is the transmission electron microscope picture of the carbon nano dot of the embodiment of the invention 1.
Fig. 2 be in the atomic power scanned picture a of carbon nano dot of the embodiment of the invention 1 and the atomic power scanned picture A to the altitude curve b of B position.
Fig. 3 is the infrared spectrogram that sees through of the carbon nano dot of the embodiment of the invention 1; At 3100-3500 cm
-1The absorption band at place is the absorption vibrational band of ν (O-H) and ν (N-H), 1600-1770 cm
-1Be the absorption vibrational band of ν (C=O), show that prepared carbon nano dot surface contains abundant amide group and carboxyl.
The preparation of carbon nano dot of the present invention:
1. 3 gram urea and 3 gram citric acids are dissolved in 10 ml waters;
2. 1. prepared urea and lemon aqueous acid are placed in the microwave oven, through 500W power microwave heating 10 minutes, obtain the brownish black solid;
3. the brownish black solid with preparation is placed in the vacuum drying oven, and vacuum tightness is 0.01 handkerchief, and temperature is 60 degrees centigrade, heats 1 hour, removes residual micromolecular compound, obtains the carbon nano dot.
The preparation of carbon nano dot of the present invention:
1. 0.3 gram urea and 3 gram citric acids are dissolved in 10 ml waters;
2. 1. prepared urea and lemon aqueous acid are placed in the microwave oven, through 700W power microwave heating 4 minutes, obtain the brownish black solid;
3. the brownish black solid with preparation is placed in the vacuum drying oven, and vacuum tightness is 0.01 handkerchief, and temperature is 50 degrees centigrade, heats 2 hours, removes residual micromolecular compound, obtains the carbon nano dot.
The preparation of carbon nano dot of the present invention:
1. 0.3 gram urea and 3 gram citric acids are dissolved in 10 ml waters;
2. 1. prepared urea and lemon aqueous acid are placed in the microwave oven, through 700W power microwave heating 4 minutes, obtain the brownish black solid;
3. the brownish black solid with preparation is placed in the vacuum drying oven, and vacuum tightness is 0.001 handkerchief, and temperature is 60 degrees centigrade, heats 1 hour, removes residual micromolecular compound, obtains the carbon nano dot.
The preparation of carbon nano dot of the present invention:
1. 6 gram urea and 3 gram citric acids are dissolved in 10 ml waters;
2. 1. prepared urea and lemon aqueous acid are placed in the microwave oven, through 900W power microwave heating 3 minutes, obtain the brownish black solid;
3. the brownish black solid with preparation is placed in the vacuum drying oven, and vacuum tightness is 0.01 handkerchief, and temperature is 55 degrees centigrade, heats 2 hours, removes residual micromolecular compound, obtains the carbon nano dot.
The preparation of carbon nano dot of the present invention:
1. 12 gram urea and 3 gram citric acids are dissolved in 15 ml waters;
2. 1. prepared urea and lemon aqueous acid are placed in the microwave oven, through 700W power microwave heating 5 minutes, obtain the brownish black solid;
3. the brownish black solid with preparation is placed in the vacuum drying oven, and vacuum tightness is 0.01 handkerchief, and temperature is 70 degrees centigrade, heats 1 hour, removes residual micromolecular compound, obtains the carbon nano dot.
The preparation of carbon nano dot of the present invention:
1. 12 gram urea and 3 gram citric acids are dissolved in 10 ml waters;
2. 1. prepared urea and lemon aqueous acid are placed in the microwave oven, through 500W power microwave heating 9 minutes, obtain the brownish black solid;
3. the brownish black solid with preparation is placed in the vacuum drying oven, and vacuum tightness is 0.1 handkerchief, and temperature is 60 degrees centigrade, heats 1 hour, removes residual micromolecular compound, obtains the carbon nano dot.
The preparation of carbon nano dot of the present invention:
1. 3 gram urea and 3 gram glycerine are dissolved in 12 ml waters;
2. 1. prepared urea and the aqueous solution of glycerine are placed in the microwave oven, through 600W power microwave heating 8 minutes, obtain the brownish black solid;
3. the brownish black solid with preparation is placed in the vacuum drying oven, and vacuum tightness is 0.05 handkerchief, and temperature is 55 degrees centigrade, heats 2 hours, removes residual micromolecular compound, obtains the carbon nano dot.
Embodiment 9
The preparation of carbon nano dot of the present invention:
1. 3 gram urea and 3 gram glucose are dissolved in 12 ml waters;
2. 1. prepared urea and the aqueous solution of glucose are placed in the microwave oven, through 600W power microwave heating 8 minutes, obtain the brownish black solid;
3. the brownish black solid with preparation is placed in the vacuum drying oven, and vacuum tightness is 0.01 handkerchief, and temperature is 60 degrees centigrade, heats 1 hour, removes residual micromolecular compound, obtains the carbon nano dot.
Embodiment 10
The preparation of carbon nano dot of the present invention:
1. 3 gram urea and 3 gram sucrose dissolved are in 15 ml waters;
2. 1. prepared urea and the aqueous solution of sucrose are placed in the microwave oven, through 700W power microwave heating 6 minutes, obtain the brownish black solid;
3. the brownish black solid with preparation is placed in the vacuum drying oven, and vacuum tightness is 0.01 handkerchief, and temperature is 70 degrees centigrade, heats 1 hour, removes residual micromolecular compound, obtains the carbon nano dot.
Embodiment 11
The preparation of carbon nano dot of the present invention:
1. 3 gram urea and 3 gram glycine are dissolved in 10 ml waters;
2. 1. prepared urea and the aqueous solution of glycine are placed in the microwave oven, through 700W power microwave heating 7 minutes, obtain the brownish black solid;
3. the brownish black solid with preparation is placed in the vacuum drying oven, and vacuum tightness is 0.01 handkerchief, and temperature is 60 degrees centigrade, heats 2 hours, removes residual micromolecular compound, obtains the carbon nano dot.
Embodiment 12-22 is the Application Example of carbon nano dot of the present invention in the preparation fluorescent ink.
Embodiment 12
In conjunction with Fig. 4-13 explanation present embodiment
The application of carbon nano dot of the present invention in the preparation fluorescent ink:
The carbon nano dot that embodiment 1 is obtained is dissolved in 100 ml waters, and through centrifugal treating, 3000 rev/mins of centrifugal rotational speeds, centrifugation time 20 minutes obtains supernatant liquor; The supernatant liquor that obtains dilutes through water, and obtaining concentration is the aqueous solution of the carbon nano dot of 1 mg/ml, i.e. carbon nano dot fluorescent ink.
The prepared permanent placement of carbon nano dot fluorescent ink can not produce precipitation.
Fig. 4 is the ultra-violet absorption spectrum and fluorescence emission spectrogram under different excitation wavelengths of the aqueous solution of the carbon nano dot of the embodiment of the invention 12: curve 1 is uv absorption spectra, curve 2 is the fluorescence emission spectrogram of 340nm under exciting, curve 3 is the fluorescence emission spectrogram of 380nm under exciting, curve 4 is the fluorescence emission spectrogram of 420nm under exciting, curve 5 is the fluorescence emission spectrogram of 460nm under exciting, and curve 6 is the fluorescence emission spectrogram of 500nm under exciting; Excitation wavelength is that hyperfluorescenceCeng Yongminggaoyingguang emission peak 540nm appears in 420nm as can be seen from Figure 1, and the maximum fluorescence quantum yield is 14%.
Fig. 5 is that the carbon nano dot fluorescent ink of the embodiment of the invention 12 drips on the filter paper, behind the air drying, at the fluorescence emission spectral curve under the different excitation wavelengths: the fluorescence emission spectrogram under curve 1 excites for 340nm, curve 2 is the fluorescence emission spectrogram of 380nm under exciting, curve 3 is the fluorescence emission spectrogram of 420nm under exciting, curve 4 is the fluorescence emission spectrogram of 460nm under exciting, and curve 5 is the fluorescence emission spectrogram of 500nm under exciting; Excitation wavelength is that hyperfluorescenceCeng Yongminggaoyingguang emission peak 515nm appears in 420nm as can be seen from Figure 2, and the maximum fluorescence quantum yield is 40%.
Fig. 6 is that the carbon nano dot fluorescent ink of the embodiment of the invention 12 makes growth of mung beans become to have the photo under different-waveband illumination of the bean sprouts of fluorescent characteristic: (a) photo under the natural light, (b) excitation wavelength 340 nm, receive wavelength greater than the fluorescence photo of 395 nm light, it is blue that the bean sprouts is, (c) excitation wavelength 420 nm, receive wavelength greater than the fluorescence photo of 450 nm, it is green that the bean sprouts is, (d) excitation wavelength 500 nm, receive wavelength greater than the fluorescence photo of 550 nm, it is orange that the bean sprouts is; Show with carbon nano dot fluorescent ink of the present invention nontoxicly to plant, and can dye to plant living body.
Fig. 7 is the big white mouse urine of carbon nano dot fluorescent ink in the time of one month of drinking the embodiment of the invention 12 at the fluorescence spectrum figure under the different excitation wavelengths: the fluorescence emission spectrogram under curve 1 excites for 340nm, curve 2 is the fluorescence emission spectrogram of 360nm under exciting, curve 3 is the fluorescence emission spectrogram of 380nm under exciting, curve 4 is the fluorescence emission spectrogram of 400nm under exciting, curve 5 is the fluorescence emission spectrogram of 420nm under exciting, curve 6 is the fluorescence emission spectrogram of 460nm under exciting, curve 7 is the fluorescence emission spectrogram of 480nm under exciting, curve 8 is the fluorescence emission spectrogram of 500nm under exciting, and the fluorescent band that 500-600 nm place occurs shows and contains the prepared carbon nano dot of the present invention in the urine.
Fig. 8 is that big white mouse was drunk the carbon nano dot fluorescent ink of the embodiment of the invention 12 after one month, stop to drink carbon nano dot fluorescent ink of the present invention, change and drink the urine of normal tap water in the time of 1 month at the fluorescence spectrum figure under the different excitation wavelengths: the fluorescence emission spectrogram under curve 1 excites for 340nm, curve 2 is the fluorescence emission spectrogram of 360nm under exciting, curve 3 is the fluorescence emission spectrogram of 380nm under exciting, curve 4 is the fluorescence emission spectrogram of 400nm under exciting, curve 5 is the fluorescence emission spectrogram of 420nm under exciting, curve 6 is the fluorescence emission spectrogram of 460nm under exciting, and the fluorescent band that 500-600 nm place occurs disappears.
Fig. 9 is that big white mouse is drunk the urine of normal tap water (not drinking carbon nano dot fluorescent ink of the present invention) at the fluorescence spectrum figure of different excitation wavelengths: the fluorescence emission spectrogram under curve 1 excites for 340nm, curve 2 is the fluorescence emission spectrogram of 360nm under exciting, curve 3 is the fluorescence emission spectrogram of 380nm under exciting, curve 4 is the fluorescence emission spectrogram of 400nm under exciting, curve 5 is the fluorescence emission spectrogram of 420nm under exciting, and curve 6 is the fluorescence emission spectrogram of 460nm under exciting.
Fig. 7-9 shows that the big white mouse long-term drinking carbon nano dot fluorescent ink with citric acid and urea preparation of the present invention can not cause death or produce unusual phenomenon, and carbon nano dot fluorescent ink of the present invention can be discharged through urine, and is nontoxic to animal.
Figure 10 is the carbon nano dot fluorescent ink of the embodiment of the invention 12 and commercial green fluorescence pen (be purchased and get final product) consists of enciphered digital at paper fluorescence photo: write " 395 " at paper with carbon nano dot fluorescent ink, do not smear and write the place with carbon nano dot fluorescent ink to be purchased the green fluorescence pen again, " 395 " are mended into numeral " 888 "; A figure, excitation wavelength 450-480 nm receives wavelength greater than the light of 515 nm, 50 milliseconds of time shutter; B figure, excitation wavelength 510-550 nm receives wavelength greater than the light of 590 nm, 150 milliseconds of time shutter; Can find out that a figure shows what show for green 888, b figure be redness 395, show that carbon nano dot fluorescent ink of the present invention can both manifest under different excitation wavelengths, can be used for enciphered digital.
Figure 11 is the cotton thread and the photo of nylon fiber under different excitation wavelengths of being infected with the carbon nano dot fluorescent ink of not being infected with the embodiment of the invention 12: cotton thread and the nylon fiber of not being infected with the carbon nano dot fluorescent ink of the embodiment of the invention 12, (a) optical photograph, (b) excitation wavelength 450-480 nm, receive wavelength greater than the fluorescence photo of 515 nm light, 50 milliseconds of time shutter, (c) excitation wavelength 510-550 nm, receive wavelength greater than the fluorescence photo of 590 nm light, 150 milliseconds of time shutter; Be infected with the carbon nano dot fluorescent ink of the embodiment of the invention 12, and (d) optical photograph of the cotton thread behind air drying and nylon fiber, (e) excitation wavelength 450-480 nm, receive wavelength greater than the fluorescence photo of 515 nm, 50 milliseconds of time shutter, can find out that cotton fibre is green, (f) excitation wavelength 510-550 nm, receive wavelength greater than the fluorescence photo of 590 nm light, 150 milliseconds of time shutter, can find out that cotton fibre takes on a red color; As can be seen from Figure 11, the cotton fibre of being infected with the carbon nano dot fluorescent ink of the embodiment of the invention 12 shows the fluorescence phenomenon that strong excitation wavelength relies on, and the nylon fiber of being infected with the carbon nano dot fluorescent ink of the embodiment of the invention 12 does not have fluorescence phenomenon, shows that carbon nano dot fluorescent ink of the present invention can identify biological product and Chemicals effectively.
Figure 12 uses the carbon nano dot fluorescent ink of the embodiment of the invention 12 at the photo of fingerprints mark under different excitation wavelengths on the paper, (a) optical photograph, (b) excitation wavelength 340 nm, receive wavelength greater than the fluorescence photo of 395 nm light, can find out that (b) figure manifests blue fingerprint, (c) excitation wavelength 420 nm receive wavelength greater than the fluorescence photo of 450 nm light, can find out (c) figure shows green fingerprint; The fingerprint that obtains can be preserved for a long time.
Figure 13 is the carbon nano dot fluorescent ink of the embodiment of the invention 12 stays fluorescent graphic at skin fluorescence photo.
Embodiment 13
In conjunction with Figure 14 embodiment 13 is described
The application of carbon nano dot of the present invention in the preparation fluorescent ink:
The carbon nano dot that embodiment 2 is obtained is dissolved in 200 milliliters of ethanol, and through centrifugal treating, 3000 rev/mins of centrifugal rotational speeds, centrifugation time 20 minutes obtains supernatant liquor; The supernatant liquor that obtains is through alcohol dilution, and obtaining concentration is the ethanolic soln of the carbon nano dot of 1 mg/ml, i.e. carbon nano dot fluorescent ink.
Figure 14 be the ethanolic soln of carbon nano dot of the embodiment of the invention 13 at the fluorescence emission spectrogram under the different excitation wavelengths: the fluorescence emission spectrogram under curve 1 excites for 340nm, curve 2 is the fluorescence emission spectrogram of 380nm under exciting, curve 3 is the fluorescence emission spectrogram of 420nm under exciting, curve 4 is the fluorescence emission spectrogram of 460nm under exciting, and curve 5 is the fluorescence emission spectrogram of 500nm under exciting; HyperfluorescenceCeng Yongminggaoyingguang emission peak 520nm (excitation wavelength 420nm), the maximum fluorescence quantum yield is 38%.
Embodiment 14
In conjunction with Figure 15,16 explanation embodiment 14
The application of carbon nano dot of the present invention in the preparation fluorescent ink:
The carbon nano dot that embodiment 3 is obtained is dissolved in 100 ml waters, and through centrifugal treating, 2000 rev/mins of centrifugal rotational speeds, centrifugation time 30 minutes obtains supernatant liquor; The supernatant liquor that obtains dilutes through water, and obtaining concentration is the aqueous solution of the carbon nano dot of 1 mg/ml, i.e. carbon nano dot fluorescent ink.
Figure 15 be the aqueous solution of carbon nano dot of the embodiment of the invention 14 at the fluorescence emission spectrogram under the different excitation wavelengths: the fluorescence emission spectrogram under curve 1 excites for 320nm, curve 2 is the fluorescence emission spectrogram of 360nm under exciting, curve 3 is the fluorescence emission spectrogram of 380nm under exciting, curve 4 is the fluorescence emission spectrogram of 390nm under exciting, curve 5 is the fluorescence emission spectrogram of 400nm under exciting, and curve 6 is the fluorescence emission spectrogram of 460nm under exciting; HyperfluorescenceCeng Yongminggaoyingguang emission peak 445nm (excitation wavelength 360nm) maximum fluorescence quantum yield is 18%.
Figure 16 is that the carbon nano dot fluorescent ink of the embodiment of the invention 14 drips on the filter paper, and behind air drying, at the fluorescence emission spectrogram under the different excitation wavelengths: the fluorescence emission spectrogram under curve 1 excites for 320nm, curve 2 is the fluorescence emission spectrogram of 360nm under exciting, curve 3 is the fluorescence emission spectrogram of 380nm under exciting, curve 4 is the fluorescence emission spectrogram of 400nm under exciting, curve 5 is the fluorescence emission spectrogram of 420nm under exciting, and curve 6 is the fluorescence emission spectrogram of 480nm under exciting; HyperfluorescenceCeng Yongminggaoyingguang emission peak 443nm (excitation wavelength 360nm), the maximum fluorescence quantum yield is 18%.
Embodiment 15
In conjunction with Figure 17 embodiment 15 is described
The application of carbon nano dot of the present invention in the preparation fluorescent ink:
The carbon nano dot that embodiment 4 is obtained is dissolved in 100 milliliters of ethanol, and through centrifugal treating, 3000 rev/mins of centrifugal rotational speeds, centrifugation time 25 minutes obtains supernatant liquor; The supernatant liquor that obtains is through alcohol dilution, and obtaining concentration is the ethanolic soln of the carbon nano dot of 1 mg/ml, i.e. carbon nano dot fluorescent ink.
Figure 17 be the ethanolic soln of carbon nano dot of the embodiment of the invention 15 at the fluorescence emission spectrogram under the different excitation wavelengths: the fluorescence emission spectrogram under curve 1 excites for 320nm, curve 2 is the fluorescence emission spectrogram of 360nm under exciting, curve 3 is the fluorescence emission spectrogram of 380nm under exciting, curve 4 is the fluorescence emission spectrogram of 420nm under exciting, curve 5 is the fluorescence emission spectrogram of 460nm under exciting, and curve 6 is the fluorescence emission spectrogram of 500nm under exciting; HyperfluorescenceCeng Yongminggaoyingguang emission peak 467nm (excitation wavelength 380nm), the maximum fluorescence quantum yield is 18%.
Embodiment 16
In conjunction with Figure 18 embodiment 16 is described
The application of carbon nano dot of the present invention in the preparation fluorescent ink:
The carbon nano dot that embodiment 5 is obtained is dissolved in 100 ml waters, and through centrifugal treating, 4000 rev/mins of centrifugal rotational speeds, centrifugation time 16 minutes obtains supernatant liquor; The supernatant liquor that obtains dilutes through water, and obtaining concentration is the aqueous solution of the carbon nano dot of 1 mg/ml, i.e. carbon nano dot fluorescent ink.
Figure 18 be the aqueous solution of carbon nano dot of the embodiment of the invention 16 at the fluorescence emission spectrogram under the different excitation wavelengths: the fluorescence emission spectrogram under curve 1 excites for 320nm, curve 2 is the fluorescence emission spectrogram of 360nm under exciting, curve 3 is the fluorescence emission spectrogram of 380nm under exciting, curve 4 is the fluorescence emission spectrogram of 390nm under exciting, curve 5 is the fluorescence emission spectrogram of 400nm under exciting, and curve 6 is the fluorescence emission spectrogram of 460nm under exciting; HyperfluorescenceCeng Yongminggaoyingguang emission peak 535nm (excitation wavelength 420nm), the maximum fluorescence quantum yield is 18%.
Embodiment 17
In conjunction with Figure 19,20 explanation embodiment 17
The application of carbon nano dot of the present invention in the preparation fluorescent ink:
The carbon nano dot that embodiment 6 is obtained is dissolved in 100 ml waters, and through centrifugal treating, 3000 rev/mins of centrifugal rotational speeds, centrifugation time 20 minutes obtains supernatant liquor; The supernatant liquor that obtains dilutes through water, and obtaining concentration is the aqueous solution of the carbon nano dot of 1 mg/ml, i.e. carbon nano dot fluorescent ink.
Figure 19 be the aqueous solution of carbon nano dot of the embodiment of the invention 17 at the fluorescence emission spectrogram under the different excitation wavelengths: the fluorescence emission spectrogram under curve 1 excites for 350nm, curve 2 is the fluorescence emission spectrogram of 360nm under exciting, curve 3 is the fluorescence emission spectrogram of 380nm under exciting, curve 4 is the fluorescence emission spectrogram of 420nm under exciting, curve 5 is the fluorescence emission spectrogram of 460nm under exciting, curve 6 is the fluorescence emission spectrogram of 480nm under exciting, and curve 7 is the fluorescence emission spectrogram of 500nm under exciting; HyperfluorescenceCeng Yongminggaoyingguang emission peak 535nm (excitation wavelength 420nm) maximum fluorescence quantum yield is 18%.
Figure 20 is that the carbon nano dot fluorescent ink of the embodiment of the invention 17 drips on the filter paper, and behind air drying, at the fluorescence emission spectrogram under the different excitation wavelengths: the fluorescence emission spectrogram under curve 1 excites for 320nm, curve 2 is the fluorescence emission spectrogram of 360nm under exciting, curve 3 is the fluorescence emission spectrogram of 380nm under exciting, curve 4 is the fluorescence emission spectrogram of 420nm under exciting, curve 5 is the fluorescence emission spectrogram of 460nm under exciting, and curve 6 is the fluorescence emission spectrogram of 480nm under exciting; HyperfluorescenceCeng Yongminggaoyingguang emission peak 520nm (excitation wavelength 420nm), the maximum fluorescence quantum yield is 42%.
Embodiment 18
In conjunction with Figure 21 embodiment 18 is described
The application of carbon nano dot of the present invention in the preparation fluorescent ink:
The carbon nano dot that embodiment 7 is obtained is dissolved in 100 milliliters of ethanol, and through centrifugal treating, 3000 rev/mins of centrifugal rotational speeds, centrifugation time 22 minutes obtains supernatant liquor; The supernatant liquor that obtains is through alcohol dilution, and obtaining concentration is the ethanolic soln of the carbon nano dot of 1 mg/ml, i.e. carbon nano dot fluorescent ink.
Figure 21 be the ethanolic soln of carbon nano dot of the embodiment of the invention 18 at the fluorescence emission spectrogram under the different excitation wavelengths: the fluorescence emission spectrogram under curve 1 excites for 340nm, curve 2 is the fluorescence emission spectrogram of 380nm under exciting, curve 3 is the fluorescence emission spectrogram of 420nm under exciting, curve 4 is the fluorescence emission spectrogram of 460nm under exciting, and curve 5 is the fluorescence emission spectrogram of 500nm under exciting; HyperfluorescenceCeng Yongminggaoyingguang emission peak 527nm (excitation wavelength 420nm), the maximum fluorescence quantum yield is 40%.
Embodiment 19
In conjunction with Figure 22 embodiment 19 is described
The application of carbon nano dot of the present invention in the preparation fluorescent ink:
The carbon nano dot that embodiment 8 is obtained is dissolved in 100 ml waters, and through centrifugal treating, 3000 rev/mins of centrifugal rotational speeds, centrifugation time 25 minutes obtains supernatant liquor; The supernatant liquor that obtains dilutes through water, and obtaining concentration is the aqueous solution of the carbon nano dot of 1 mg/ml, i.e. carbon nano dot fluorescent ink.
Figure 22 be the aqueous solution of carbon nano dot of the embodiment of the invention 19 at the fluorescence emission spectrogram under the different excitation wavelengths: the fluorescence emission spectrogram under curve 1 excites for 300nm, curve 2 is the fluorescence emission spectrogram of 340nm under exciting, curve 3 is the fluorescence emission spectrogram of 380nm under exciting, curve 4 is the fluorescence emission spectrogram of 420nm under exciting, curve 5 is the fluorescence emission spectrogram of 450nm under exciting, and curve 6 is the fluorescence emission spectrogram of 480nm under exciting; HyperfluorescenceCeng Yongminggaoyingguang emission peak 428nm (excitation wavelength 340nm), the maximum fluorescence quantum yield is 10%.
In conjunction with Figure 23 embodiment 20 is described
The application of carbon nano dot of the present invention in the preparation fluorescent ink:
The carbon nano dot that embodiment 9 is obtained is dissolved in 100 ml waters, and through centrifugal treating, 4000 rev/mins of centrifugal rotational speeds, centrifugation time 20 minutes obtains supernatant liquor; The supernatant liquor that obtains dilutes through water, and obtaining concentration is the aqueous solution of the carbon nano dot of 1 mg/ml, i.e. carbon nano dot fluorescent ink.
Figure 23 be the aqueous solution of carbon nano dot of the embodiment of the invention 20 at the fluorescence emission spectrogram under the different excitation wavelengths: the fluorescence emission spectrogram under curve 1 excites for 300nm, curve 2 is the fluorescence emission spectrogram of 340nm under exciting, curve 3 is the fluorescence emission spectrogram of 380nm under exciting, curve 4 is the fluorescence emission spectrogram of 420nm under exciting, curve 5 is the fluorescence emission spectrogram of 450nm under exciting, and curve 6 is the fluorescence emission spectrogram of 480nm under exciting; HyperfluorescenceCeng Yongminggaoyingguang emission peak 420nm (excitation wavelength 340nm), the maximum fluorescence quantum yield is 8%.
Embodiment 21
In conjunction with Figure 24 embodiment 21 is described
The application of carbon nano dot of the present invention in the preparation fluorescent ink:
The carbon nano dot that embodiment 10 is obtained is dissolved in 100 ml waters, and through centrifugal treating, 3000 rev/mins of centrifugal rotational speeds, centrifugation time 20 minutes obtains supernatant liquor; The supernatant liquor that obtains dilutes through water, and obtaining concentration is the aqueous solution of the carbon nano dot of 1 mg/ml, i.e. carbon nano dot fluorescent ink.
Figure 24 be the aqueous solution of carbon nano dot of the embodiment of the invention 21 at the fluorescence emission spectrogram under the different excitation wavelengths: the fluorescence emission spectrogram under curve 1 excites for 320nm, curve 2 is the fluorescence emission spectrogram of 360nm under exciting, curve 3 is the fluorescence emission spectrogram of 400nm under exciting, curve 4 is the fluorescence emission spectrogram of 440nm under exciting, and curve 5 is the fluorescence emission spectrogram of 480nm under exciting; HyperfluorescenceCeng Yongminggaoyingguang emission peak 425nm (excitation wavelength 400nm), the maximum fluorescence quantum yield is 6%.
Embodiment 22
In conjunction with Figure 25 embodiment 22 is described
The application of carbon nano dot of the present invention in the preparation fluorescent ink:
The carbon nano dot that embodiment 11 is obtained is dissolved in 100 ml waters, and through centrifugal treating, 3000 rev/mins of centrifugal rotational speeds, centrifugation time 20 minutes obtains supernatant liquor; The supernatant liquor that obtains dilutes through water, and obtaining concentration is the aqueous solution of the carbon nano dot of 1 mg/ml, i.e. carbon nano dot fluorescent ink.
Figure 25 be the aqueous solution of carbon nano dot of the embodiment of the invention 22 at the fluorescence emission spectrogram under the different excitation wavelengths: the fluorescence emission spectrogram under curve 1 excites for 300nm, curve 2 is the fluorescence emission spectrogram of 320nm under exciting, curve 3 is the fluorescence emission spectrogram of 340nm under exciting, curve 4 is the fluorescence emission spectrogram of 360nm under exciting, curve 5 is the fluorescence emission spectrogram of 380nm under exciting, curve 6 is the fluorescence emission spectrogram of 420nm under exciting, and curve 7 is the fluorescence emission spectrogram of 460nm under exciting; HyperfluorescenceCeng Yongminggaoyingguang emission peak 390nm (excitation wavelength 340nm), the maximum fluorescence quantum yield is 12%.
Claims (10)
1. a carbon nano dot is characterized in that, this carbon nano dot is to contain many carboxyls or polyhydric organic compound is raw material, or take amino acid as raw material, is prepared from take urea as the surface passivation agent, and step is as follows:
1. urea with contain many carboxyls or polyhydric organic compound, or amino acid in mass ratio 0.1:1-4:1 be mixed with the aqueous solution;
2. the 1. prepared aqueous solution is obtained the brownish black solid by the microwave heating reaction;
3. the brownish black solid that obtains is removed residual micromolecular compound through heating under vacuum, namely obtains the carbon nano dot.
2. a kind of carbon nano dot according to claim 1 is characterized in that, described many carboxyls or polyhydric organic compound are citric acid, ethylenediamine tetraacetic acid (EDTA), glycerine, glucose, fructose, sucrose, chitosan or starch.
3. a kind of carbon nano dot according to claim 1 is characterized in that, described amino acid is glycine or L-glutamic acid.
4. a kind of carbon nano dot according to claim 1 is characterized in that, step 1. in, described urea with contain many carboxyls or polyhydric organic compound, or amino acid in mass ratio 0.1:1-4:1 be mixed with saturated aqueous solution.
5. a kind of carbon nano dot according to claim 1 is characterized in that, step 2. in, the described aqueous solution was through 500-900W power microwave heating 3-10 minute.
6. a kind of carbon nano dot according to claim 1 is characterized in that, step 3. in, the vacuum tightness of described heating under vacuum is the 0.001-0.1 handkerchief, Heating temperature is 50-70 degree centigrade, 1-2 hour heat-up time.
7. the preparation method of a carbon nano dot is characterized in that, may further comprise the steps:
1. urea with contain many carboxyls or polyhydric organic compound, or amino acid in mass ratio 0.1:1-4:1 be mixed with the aqueous solution;
2. the 1. prepared aqueous solution is obtained the brownish black solid by the microwave heating reaction;
3. with the brownish black solid through heating under vacuum, remove residual micromolecular compound, obtain the carbon nano dot.
8. the application of any one described a kind of carbon nano dot of claim 1-6 in the preparation fluorescent ink.
9. the application of a kind of carbon nano dot according to claim 8 in the preparation fluorescent ink is characterized in that, the carbon nano dot is soluble in water, through centrifugal, obtains supernatant liquor; The supernatant liquor that obtains through water or organic solvent diluting, is obtained carbon nano dot fluorescent ink.
10. the application of a kind of carbon nano dot according to claim 9 in the preparation fluorescent ink is characterized in that centrifugal rotational speed is 2000-4000 rev/min, and the time is 15-30 minute.
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