CN107325815A - High quantum production rate fluorescent carbon point of N doping and its preparation method and application - Google Patents
High quantum production rate fluorescent carbon point of N doping and its preparation method and application Download PDFInfo
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Abstract
The present invention relates to high quantum production rate fluorescent carbon point of N doping and its preparation method and application.The technical scheme of use is：Malic acid and ammonium phosphate are put into the reactor of inner liner polytetrafluoroethylene by a certain percentage, at 180~230 DEG C, heating 4~9 hours, naturally cool to room temperature and obtain the solution that dark-brown contains carbon point, then the carbon dots solution purified by high speed centrifugation, filtering and dialysis, finally be freeze-dried obtaining fluorescent carbon point solid powder.The present invention uses fusion method using malic acid as carbon source, and ammonium phosphate is nitrogen source, one-step synthesis fluorescent carbon point.This method prepares that carbon point raw material is easy to get, method is simple, yield is high, synthesis condition gentle carbon point good water solubility, stability controllable, prepare is good, fluorescence quantum yield is high and the fluorescence of sapphirine is presented under ultraviolet light.
Description
Technical field
The present invention relates to carbon nanomaterial technical field.Specifically related to a kind of high quantum production rate of N doping, ultraviolet
Light irradiation issues fluorescent carbon point of light blue coloured light and its preparation method and application.
Background technology
Carbon point (Carbon Dots) is the novel fluorescence nano-particle that a kind of diameter is less than 10nm.Fluorescent carbon point, which has, to swash
Send out wavelength and launch wavelength is tunable, fluorescence property is stable, the good luminescent properties of fast light Bleachability grade.Meanwhile, the grain of carbon point
Footpath and the equal very little of molecular weight, good biocompatibility.Carbon point can enter cell interior without influenceing nucleus by cell endocytic,
Can also be with DNA interaction of biomacromolecules, so that identification and detection to carry out DNA, so carbon point can apply to carefully
In terms of born of the same parents' imaging and biomarker.In addition, fluorescent carbon point also has some special properties in itself, make it in photocatalytic degradation
In terms of also have good application prospect.The carbon point fluorescence quantum yield for generally comprising only hydroxyl and carboxyl is relatively low, and nitrogen is mixed
Miscellaneous is a kind of one of effective method for improving carbon point luminous efficiency.Therefore, it is necessary to find it is a kind of quickly, it is simple, with
Cheap raw material is carbon source, synthesizes a kind of method of the fluorescent carbon point of high quantum production rate.
The content of the invention
It is an object of the invention to provide a kind of method is simple, effective, fluorescence quantum yield is high, N doping, in uviol lamp
Irradiation issues the preparation method of the fluorescent carbon point of light blue coloured light.
To realize the purpose of the present invention, the technical solution adopted by the present invention is as follows：The high quantum production rate fluorescent carbon of N doping
Point, preparation method comprises the following steps：Proper amount of carbon source and nitrogen source are put into inner liner polytetrafluoroethylene reactor, 180~230
At DEG C, 4~9h is heated, room temperature is naturally cooled to, added after ultra-pure water dilution, high speed centrifugation, then with 0.22 μm of filter mistake
Filter, dialysis, freeze-drying, obtain the high quantum production rate fluorescent carbon point powder of N doping.
The high quantum production rate fluorescent carbon point of above-mentioned N doping, described carbon source is malic acid.
The high quantum production rate fluorescent carbon point of above-mentioned N doping, described nitrogen source is ammonium phosphate.
The high quantum production rate fluorescent carbon point of above-mentioned N doping, in mass ratio, carbon source:Nitrogen source=1:(0.1~1).
The high quantum production rate fluorescent carbon point of above-mentioned N doping, described high speed centrifugation is that rotating speed is 10000rpm/min.
Application of the high quantum production rate fluorescent carbon point of above-mentioned N doping in degradating organic dye.Method is as follows：Yu Han
Have in the solution of organic dyestuff, add the high quantum production rate fluorescent carbon point solution and H of above-mentioned N doping2O2, under high-pressure sodium lamp
Irradiation.
Application of the high quantum production rate fluorescent carbon point of above-mentioned N doping in bio-imaging.Method is as follows：Will be above-mentioned
The high quantum production rate fluorescent carbon point and cell of N doping are co-cultured, with the imaging effect of fluorescence microscope cell.
The beneficial effects of the invention are as follows：The present invention is that can obtain carbon point by a step fusion method, and synthesized carbon point exists
Under 365nm ultra violet lamps, sapphirine is presented.Synthetic method of the present invention is easy and effective, and raw material is cheap and easy to get, and reaction condition is gentle
It is controllable and environment-friendly, it can be completed in general laboratory, it is easy to promote.The carbon point fluorescence prepared using the inventive method
Quantum yield is up to more than 20%.
Brief description of the drawings
Fig. 1 is transmission electron microscope (TEM) photo of carbon point prepared by embodiment 1.
Fig. 2 is X-ray diffraction (XRD) figure of carbon point prepared by embodiment 1.
Fig. 3 is the infrared spectrogram of carbon point prepared by embodiment 1.
Fig. 4 a are x-ray photoelectron power spectrum (XPS) figures of carbon point prepared by embodiment 1.
Fig. 4 b are C 1s figures.
Fig. 4 c are N 1s figures.
Fig. 4 d are O 1s figures.
Fig. 5 is the UV-visible absorption spectrum of the carbon point aqueous solution prepared by embodiment 1.
Fig. 6 is the fluorescence excitation and launching light spectrogram of the carbon point aqueous solution prepared by embodiment 1.
Fig. 7 is fluorescence emission spectrogram of compound (excitation wave of the carbon point aqueous solution of the preparation of embodiment 1 in the case where different wavelengths of light is excited
Length is by 310nm to 400nm, and step-length is 10nm).
Fig. 8 is the influence for the carbon point fluorescence intensity that pH value is prepared to embodiment 1.
Fig. 9 be ionic strength to be carbon point fluorescence intensity prepared by embodiment 1 influence.
Figure 10 is the influence (365nm) for the carbon point fluorescence intensity that illumination is prepared to embodiment 1.
Figure 11 is photocatalytic degradation result of the crystal violet in the presence of carbon point prepared by embodiment 1.
Figure 12 is the percent of decolourization of the crystal violet in the presence of carbon point prepared by embodiment 1 with light application time change curve.
Figure 13 is the cell imaging of carbon point prepared by embodiment 1.
Embodiment
With reference to specific embodiment, the invention will be further described.
Embodiment 1
0.5g malic acid and 0.35g ammonium phosphate are weighed in ptfe autoclave, is well mixed, is put into forced air drying
In case, 7h is heated in 220 DEG C, room temperature is naturally cooled to, obtain the dark-brown solution containing carbon point, add 10mL ultra-pure waters dilute
Release, 5min is centrifuged with 10000rpm/min rotating speed, then filtered with 0.22 μm of filter, then dialysed, the carbon point purified is molten
Liquid, is finally freeze-dried with freeze drier, obtains the high quantum production rate fluorescent carbon point solid powder of N doping.Measure carbon point glimmering
Quantum yield is 20.7%.
The transmission electron microscope photo of the high quantum production rate fluorescent carbon point of the N doping of preparation is as shown in Figure 1.As seen from Figure 1, carbon
The particle diameter of point is in 5nm or so, favorable dispersibility.
The X-ray diffractogram of the high quantum production rate fluorescent carbon point of the N doping of preparation is as shown in Figure 2.From Figure 2 it can be seen that carbon point
There is one in the range of 2 θ=10 °~60 ° it will be evident that very wide diffraction maximum, this is the characteristic peak of agraphitic carbon.
The infrared spectrogram of the high quantum production rate fluorescent carbon point of the N doping of preparation is as shown in Figure 3.As seen from Figure 3,
3419cm-1Absworption peak belongs to N-H/O-H stretching vibration peak；1397cm-1The in-plane bending that place's absworption peak belongs to O-H shakes
It is dynamic；2927cm-1Place's absworption peak belongs to C-H stretching vibration；1610cm-1The C that the small absworption peak in place is belonged on aromatic ring frame
=C stretching vibrations；1714cm-1Place's absworption peak carrys out the stretching vibration as the C=O in carboxyl；1187cm-1Locate absworption peak ownership
In C-O-C/C-N stretching vibration；1051cm-1The small absworption peak at place belongs to O-H and N-H stretching vibration；950cm-1Place
Small peak absworption peak belongs to P-O-C flexural vibrations, also illustrates to contain phosphorus in carbon point, but seldom.
The XPS spectrum figure of the high quantum production rate fluorescent carbon point of the N doping of preparation is as shown in figures 4a-4d.From Fig. 4 a, this
Carbon point contains the elements such as C, N, O, illustrates that N has successfully been doped in carbon point；From Fig. 4 b, the C1s of carbon point 282eV,
There is obvious absworption peak at 282.8eV, 284.0eV and 288.6eV, represent four kinds of different compositions belonging to carbon, it is right respectively
Should be in the presence of the groups such as C-H, C-O, C=C, C=O；From Fig. 4 c, the N1s of carbon point has at 397.5eV and 398.3eV
Obvious absworption peak, represents two kinds of different compositions of nitrogen, corresponds respectively to the presence of the groups such as C-N and N-H；Can by Fig. 4 d
Know, the O1s of carbon point has obvious absworption peak at 529eV, 529.9eV and 530.9eV, represent three kinds of different groups of oxygen element
Into corresponding respectively to the presence of the groups such as C=O, C-O and O-H.
The uv-visible absorption spectra of the high quantum production rate fluorescent carbon point of the N doping of preparation is as shown in Figure 5.Can by Fig. 5
See, carbon point has obvious characteristic absorption peak at 340nm, corresponding to C=O n → π * transition.
The fluorescence excitation and emission spectrum of the high quantum production rate fluorescent carbon point of the N doping of preparation are as shown in Figure 6.Can by Fig. 6
See, the maximum excitation wavelength and maximum emission wavelength of the fluorescent carbon point of N doping are respectively 370nm and 445nm.
Excite the fluorescence emission spectrum of lower fluorescent carbon point as shown in Figure 7 in different wavelengths of light.As seen from Figure 7, with exciting
Wavelength increases (from 310nm to 400nm), fluorescence emission peak gradually red shift, it is indicated that prepared carbon point has excitation wavelength dependence
Property.
Influence of the pH value to carbon point fluorescence intensity is as shown in Figure 8.As seen from Figure 8, when pH value is 3, the fluorescence of carbon point is strong
Degree is most strong, and with the increase of pH value, fluorescence intensity is gradually reduced.
Influence of the ionic strength to carbon point fluorescence intensity is as shown in Figure 9.As seen from Figure 9, with the increase of NaCl concentration, carbon
The fluorescence intensity of point is held essentially constant, it is indicated that prepared carbon point has higher saline-alkaline tolerance.
Influence of the illumination to carbon point fluorescence intensity is as shown in Figure 10.As seen from Figure 10, under 365nm ultraviolet lights, with
The increase of irradiation time, the fluorescence intensity of carbon point is held essentially constant, illustrate that prepared carbon point has stronger anti-light drift
Bai Nengli.
Embodiment 2
Weigh 0.5g malic acid and 0.2g ammonium phosphate to be well mixed in ptfe autoclave, 7h heated in 220 DEG C,
Room temperature is naturally cooled to, the dark-brown carbon point of liquid is obtained, added after the dilution of 10mL ultra-pure waters, with 10000rpm/min rotating speed
5min is centrifuged, then is filtered with 0.22 μm of filter, the carbon dots solution purified after then dialysing is finally dried with freeze drier
Obtain the fluorescent carbon point solid powder of N doping.
Embodiment 3
Weigh 0.5g malic acid and 0.25g ammonium phosphate to be well mixed in ptfe autoclave, in 220 DEG C of heating
7h, naturally cools to room temperature, obtains the dark-brown carbon point of liquid, adds after the dilution of 10mL ultra-pure waters, with 10000rpm/min's
Rotating speed centrifuges 5min, then is filtered with 0.22 μm of filter, and the carbon dots solution purified after then dialysing finally uses freeze drier
It is dried to obtain the fluorescent carbon point solid powder of N doping.
Embodiment 4
Weigh 0.5g malic acid and 0.3g ammonium phosphate to be well mixed in ptfe autoclave, 7h heated in 220 DEG C,
Room temperature is naturally cooled to, the dark-brown carbon point of liquid is obtained, added after the dilution of 10mL ultra-pure waters, with 10000rpm/min rotating speed
5min is centrifuged, then is filtered with 0.22 μm of filter, the carbon dots solution purified after then dialysing is finally dried with freeze drier
Obtain the fluorescent carbon point solid powder of N doping.
Embodiment 5
Weigh 0.5g malic acid and 0.4g ammonium phosphate to be well mixed in ptfe autoclave, 7h heated in 220 DEG C,
Room temperature is naturally cooled to, the dark-brown carbon point of liquid is obtained, added after the dilution of 10mL ultra-pure waters, with 10000rpm/min rotating speed
5min is centrifuged, then is filtered with 0.22 μm of filter, the carbon dots solution purified after then dialysing is finally dried with freeze drier
Obtain the fluorescent carbon point solid powder of N doping.
Application of the high quantum production rate fluorescent carbon point of the N doping of embodiment 6 in crystal violet degraded
50mL (5mg/L) crystal violet solution is taken in beaker, adds prepared by the embodiment 1 that 2mL concentration is 0.5g/L
The carbon point aqueous solution, under lucifuge under the conditions of stir 30min, its uv-visible absorption spectra is surveyed in sampling, is then added 2 and is dripped H2O2
(30%), with high voltage mercury lamp radiation, a sample is taken at interval of 30min, its absorption spectrum is scanned.
As seen from Figure 11, carbon point has certain photocatalysis performance, available for degradating organic dye.
Crystal violet percent of decolourization can be calculated by below equation：
In formula：A0For the starting absorbance of crystal violet solution, A is the absorbance of different t crystal violet solution.
As shown in Figure 12, after illumination 120min, percent of decolourization reaches 21.5%.Thus illustrate that there is carbon point certain light to urge
Change activity, available for degradating organic dye.
Application of the high quantum production rate fluorescent carbon point of the N doping of embodiment 7 in bio-imaging agent
The fluorescent carbon point solution and stomach cancer cell MKN-45 that concentration is prepared for 200 μ g/L embodiment 1 are common at 37 DEG C
Culture, with intake situation of the fluorescence microscope cell to carbon point, as a result as shown in figure 13.As seen from Figure 13, it is prepared
Carbon point shows certain cell imaging effect.
Claims (9)
1. the high quantum production rate fluorescent carbon point of N doping, it is characterised in that preparation method comprises the following steps：By proper amount of carbon source and
Nitrogen source is put into the reactor of inner liner polytetrafluoroethylene, at 180~230 DEG C, is heated 4~9h, is naturally cooled to room temperature, is added
After ultra-pure water dilution, then high speed centrifugation is filtered with 0.22 μm of filter, dialysed, is freeze-dried, obtain the high quantum of N doping
Yield fluorescent carbon point powder.
2. the high quantum production rate fluorescent carbon point of N doping according to claim 1, it is characterised in that：Described carbon source is apple
Tartaric acid.
3. the high quantum production rate fluorescent carbon point of N doping according to claim 1, it is characterised in that：Described nitrogen source is phosphorus
Sour ammonium.
4. the high quantum production rate fluorescent carbon point of the N doping according to claim 1,2 or 3 any one, it is characterised in that：Press
Mass ratio, carbon source:Nitrogen source=1:(0.1~1).
5. the high quantum production rate fluorescent carbon point of the N doping according to claim 1,2 or 3 any one, it is characterised in that：Institute
The high speed centrifugation stated is that rotating speed is 10000rpm/min.
6. the high quantum production rate fluorescent carbon point of the N doping described in claim 1,2 or 3 any one is in degradating organic dye
Using.
7. application according to claim 6, it is characterised in that method is as follows：In the solution containing organic dyestuff, add
The high quantum production rate fluorescent carbon point solution and H of N doping described in claim 1,2 or 3 any one2O2, shone under high-pressure sodium lamp
Penetrate.
8. application of the high quantum production rate fluorescent carbon point of the N doping described in claim 1,2 or 3 any one in bio-imaging.
9. application according to claim 8, it is characterised in that method is as follows：By described in claim 1,2 or 3 any one
N doping high quantum production rate fluorescent carbon point and cell co-culture, with the imaging effect of fluorescence microscope cell.
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| CN112940720A (en) * | 2021-02-01 | 2021-06-11 | 郑州大学 | Nitrogen-doped carbon nanodot with high luminous efficiency and preparation method thereof |
| WO2021207807A3 (en) * | 2020-01-31 | 2022-02-17 | Fundação Universidade De Brasilia | Photosynthesis stimulator based on hybrid carbon nanoparticles, related production method and related use as nanobiostimulants and nanofertilizers in agricultural crops |
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| CN111088043A (en) * | 2019-12-18 | 2020-05-01 | 辽宁大学 | Visible light excited and long-wavelength emitted fluorescent carbon dot and preparation method and application thereof |
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