CN107151555A - A kind of controllable luminous carbon nano-particles and preparation method and application - Google Patents

A kind of controllable luminous carbon nano-particles and preparation method and application Download PDF

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CN107151555A
CN107151555A CN201710482086.XA CN201710482086A CN107151555A CN 107151555 A CN107151555 A CN 107151555A CN 201710482086 A CN201710482086 A CN 201710482086A CN 107151555 A CN107151555 A CN 107151555A
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CN107151555B (en
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刘�文
刁海鹏
李婷婷
王浩江
张�荣
孙体健
张晓瑛
弓辉
李波
魏文珑
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Shanxi Medical University
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Abstract

The invention belongs to the carbon nano-particles technical field that lights, and in particular to a kind of controllable luminous carbon nano-particles and preparation method and application.A kind of controllable luminous carbon nano-particles of the present invention, are made up of following steps:(1) fresh cloves petal is dried, it is ground into powder, 1 2g is weighed in small beaker and adds deionized water 10mL and then it is fully dissolved by adding the stirring of 0 3gNaOH solids, is added in autoclave, is put into 150 250 DEG C of baking oven pyroreaction 35 hours;(2) cooling obtains brown or dark brown solution after reaction terminates, and by centrifugation, then 0.22 μm of filter filtering dialyses 3 days, it is pure carbon nano-particles solution to obtain brown color or brown liquid in 500 1000D bag filters;(3) the carbon nano-particles solution vacuum freezedrying in step (2) is obtained into brown color or brown ceramic powder, that is, is purpose carbon nano-particles, it is soluble in water to send strong blueness or green fluorescence.

Description

A kind of controllable luminous carbon nano-particles and preparation method and application
Technical field
The invention belongs to the carbon nano-particles technical field that lights, and in particular to a kind of controllable luminous carbon nano-particles and preparation Methods and applications.
Technical background
With the generation and development of nanometer technology, carbon material big family goes from strength to strength.Carbon nano-particles are big as carbon material Newcomer in family, is a kind of unique Illuminant nanometer material, because it has particle diameter small (size is less than 10nm), toxicity It is low, good water solubility, the advantages of fluorescence property is excellent and photostability is strong and the concern for enjoying researcher.Carbon nano-particles Since (Carbon Nanoparticles, CNPs) had found first from 2004, the favor of researcher is constantly subjected to, relatively Some distinctive advantages have been embodied in traditional quantum dot (QDs) and fluorescent small molecule, including:Compared with QDs, CDs has Preferable biocompatibility and environment friendly;Compared to organic fluorescent dye, CDs have fluorescent stabilization, excitation wave spectrum width and Low cost and other advantages.
At present, many synthetic methods and material can be used for the preparation of carbon nano-particles, but still with the presence of some problems, such as Some method and steps are excessively cumbersome, and the quantum yield of some carbon nano-particles is not high, and some preparation methods, which need to be added with, to be poisoned Reagent is learned, lights and concentrates on short wavelength, the limitation of controlledly synthesis, which has limited carbon nano-particles answering in actually detected With.Therefore, the carbon nano-particles synthetic method for developing simple, quick, green and low-loss and its controllable property is very must Want.
The research of current carbon nano-particles is still in the starting stage, is worth spy the problem of also many experiments and theoretical side Rope and solution.The carbon source of more environmental protection is for example found, it is more preferable come synthesis performance by more simple and safe, easy-operating method, The luminous fluorescent carbon nano-particles of controllable preparation difference, carbon nano-particles as novel fluorescence probe biomarker and from Son, have in pH detections deeper into application.
The content of the invention
In order to overcome the shortcomings of the prior art, being used it is an object of the invention to provide a kind of simple, quick method The preparation lighted in controllable fluorescent carbon nano-particles, carbon nano-particles preparation method is easy, equipment is simple, carbon source is cheap and green Environmental protection, reaction time are short, the luminous carbon nano-particles of controlledly synthesis difference;Prepared carbon nano-particles can be applied to metal ion In terms of detection, pH detection and cell imaging, detection sensitivity, detection limit and cell imaging effect are superior to ought be above Report is offered, there is important directive significance in actual sample, biology and medical application to carbon nano-particles.
The present invention to achieve the above object and the technical scheme taken is:
A kind of controllable luminous carbon nano-particles, are made up of following steps:
(1) fresh cloves petal is dried, is ground into powder, weighed 1-2g in small beaker and to add deionized water 10mL right It is fully dissolved by adding the stirring of 0-3gNaOH solids afterwards, be added in autoclave, be put into baking oven 150-250 DEG C high Temperature reaction 3-5 hours;
(2) cooling obtains brown or dark brown solution after reaction terminates, by centrifugation, and 0.22 μm of filter is filtered, then Dialysed 3 days in 500-1000D bag filters, it is pure carbon nano-particles solution to obtain brown color or brown liquid;
(3) the carbon nano-particles solution vacuum freezedrying in step (2) is obtained into brown color or brown ceramic powder, as mesh Carbon nano-particles, it is soluble in water to send strong blueness or green fluorescence.
The preparation method of the controllable luminous carbon nano-particles of the present invention, comprises the following steps:
(1) fresh cloves petal is dried, is ground into powder, weighed 1-2g in small beaker and to add deionized water 10mL right It is fully dissolved by adding the stirring of 0-3gNaOH solids afterwards, be added in autoclave, be put into baking oven 150-250 DEG C high Temperature reaction 3-5 hours;
(2) cooling obtains brown or dark brown solution after reaction terminates, by centrifugation, and 0.22 μm of filter is filtered, then Dialysed 3 days in 500-1000D bag filters, it is pure carbon nano-particles solution to obtain brown color or brown liquid;
(3) the carbon nano-particles solution vacuum freezedrying in step (2) is obtained into brown color or brown ceramic powder, as mesh Carbon nano-particles, it is soluble in water to send strong blueness or green fluorescence.
The application of the controllable luminous carbon nano-particles of the present invention, is used to detect the Fe in the aqueous solution as fluorescence probe3+Concentration With the pH value of the aqueous solution or pass through the Fe in live cell fluorescent image checking living cells3+The pH value of concentration and living cells.
Further, the present invention is used to detect the Fe in the aqueous solution3+Fe in concentration and living cells3+During concentration, preparing The addition of NaOH solids is 0g in the step of luminous carbon nano-particles (1);PH value and living cells for detecting the aqueous solution During pH value, the addition of NaOH solids is 1-3g in (1) the step of luminous carbon nano-particles are prepared.
The present invention uses above-mentioned technical proposal, has the advantages that:
(1) operating procedure of the present invention is simple, need to only add conventional typical medicine and just can adjust the luminous of carbon nano-particles, i.e., Luminous to be moved to long wavelength, for there is critically important value in bio-sensing application, reactant is carried out in same system, It can obtain aim carbon nano-particle.
(2) raw material are lilac, are very cheap green materials, wide material sources are economic and environment-friendly.
(3) production equipment is simple, and cost is low, and reaction time is short, and yield is high.
(4) carbon nano-particles of synthesis have good water solubility, and fluorescent yield is high, and biocompatibility, good light is steady It is qualitative, it is adapted to volume production.
(5) application value is high, prepares carbon nano-particles and can be applied to metal Fe3+Ion detection, its detection sensitivity is high, inspection Rising limit is minimum in pertinent literature report;The inspection of pH value of solution is applied also for by simply regulating and controlling the carbon nano-particles of preparation Survey;The carbon nano-particles of all preparations can all be successfully applied to Fe in biomarker, living cells3+Ion and pH detections, effect Substantially,
In a word, synthesis technique of the present invention is simple to operate, and raw material sources are extensive and cheap environmental protection, and preparation condition requires low and temperature It is high with, gained carbon nano-particles yield, existing carbon nano-particles preparation method is solved because of technique and raw material limitation without regulation Modelling produce problem, the carbon nano-particles can be applied to metal ion detection, biomarker, Biological imaging, electrooptical device and The fields such as anti-fake mark.
Brief description of the drawings
Fig. 1 is that the pure carbon nano-particles obtained by embodiment 1-8 are carried out fluorescence spectrum test by the present invention, and Figure 1A, B are Embodiment 1-5 fluorogram, Fig. 1 C are embodiment 6-8 fluorescence spectra.
Fig. 2 is the ultra-violet absorption spectrum, optimal fluorescence excitation and transmitting light of the pure carbon nano-particles prepared in embodiment 2 Spectrum.
Fig. 3 is the ultra-violet absorption spectrum, optimal fluorescence excitation and transmitting light of the pure carbon nano-particles prepared in embodiment 7 Spectrum.
Fig. 4 be embodiment 2, embodiment 7 prepare pure carbon nano-particles fluorescence emission spectrum change with excitation wavelength Spectrogram.
Fig. 5 is embodiment 2, the infrared spectrogram of the pure carbon nano-particles of the preparation of embodiment 7.
Fig. 6 is embodiment 2, TEM, HRTEM and grain size distribution of the pure carbon nano-particles of the preparation of embodiment 7.
Fig. 7 is embodiment 2, the XPS spectrum figure of the pure carbon nano-particles of the preparation of embodiment 7.
Fig. 8 is embodiment 2, the XRD spectra of the pure carbon nano-particles of the preparation of embodiment 7.
Fig. 9 be embodiment 2, embodiment 7 prepare pure carbon nano-particles it is prepared by Metal Ion Selective Electrode and embodiment 2 Pure carbon nano-particles to iron ion be quenched scheme.
Figure 10 is fluorogram and different circulation time of the pure carbon nano-particles of the preparation of embodiment 7 under different pH environment Several lower change in fluorescence figures.
Figure 11 is the pure carbon nano-particles that prepare of embodiment 2, embodiment 7 to breast cancer cell MCF-7 cytotoxicity MTT experiment figure.
Figure 12 is the pure carbon nano-particles mark breast cancer cell MCF-7 and detection iron ion prepared in embodiment 2 Laser co-focusing figure.
Figure 13 is that the pure carbon nano-particles prepared in embodiment 7 mark breast cancer cell MCF-7 under different pH environment to swash The common focused view of light.
Embodiment
The present invention is described in detail with reference to embodiments, specific operating process and detailed embodiment are logical Cross embodiment to provide, single protection scope of the present invention is not limited to following examples.
Embodiment 1
Step 1, fresh cloves petal dried, is ground into powder, weighs 1g in small beaker and add deionized water 10mL, It is added in autoclave, is put into 150 DEG C of baking oven pyroreaction 4 hours;
Cooling obtains brown solution after step 2, reaction terminate, and passes through centrifugation, 0.22 μm of filter filtering, then in 500- Dialysed 3 days in 1000D bag filters, it is pure carbon nano-particles solution to obtain brown color liquid;
Step 3, the carbon nano-particles solution vacuum freezedrying in step 2 obtained into brownish-yellow powder, that is, be purpose carbon Nano-particle, it is soluble in water to send blue-fluorescence;
Step 4, will the above-mentioned fluorescent carbon nano-particles aqueous solution be freeze-dried after obtain fluorescent carbon nano-particles, its relative quantity Sub- yield (using quinine sulfate as standard) is 5.8%.
Embodiment 2
Step 1, fresh cloves petal dried, is ground into powder, weighs 1g in small beaker and add deionized water 10mL, It is added in autoclave, is put into 200 DEG C of baking oven pyroreaction 4 hours;
Cooling obtains brown solution after step 2, reaction terminate, and passes through centrifugation, 0.22 μm of filter filtering, then in 500- Dialysed 3 days in 1000D bag filters, it is pure carbon nano-particles solution to obtain brown color liquid;
Step 3, the carbon nano-particles solution vacuum freezedrying in step 2 obtained into brownish-yellow powder, that is, be purpose carbon Nano-particle, it is soluble in water to send blue-fluorescence;
Step 4, will the above-mentioned fluorescent carbon nano-particles aqueous solution be freeze-dried after obtain fluorescent carbon nano-particles, its relative quantity Sub- yield (using quinine sulfate as standard) is 12.9%.
Embodiment 3
Step 1, fresh cloves petal dried, is ground into powder, weighs 1g in small beaker and add deionized water 10mL, It is added in autoclave, is put into 250 DEG C of baking oven pyroreaction 4 hours;
Cooling obtains brown solution after step 2, reaction terminate, and passes through centrifugation, 0.22 μm of filter filtering, then in 500- Dialysed 3 days in 1000D bag filters, it is pure carbon nano-particles solution to obtain brown color liquid;
Carbon nano-particles solution vacuum freezedrying in step 2 is obtained brownish-yellow powder by step 3, i.e., received for purpose carbon Rice corpuscles, it is soluble in water to send blue-fluorescence;
Step 4 obtains fluorescent carbon nano-particles after the above-mentioned fluorescent carbon nano-particles aqueous solution is freeze-dried, its relative quantity Sub- yield (using quinine sulfate as standard) is 6.8%.
Embodiment 4
Step 1, fresh cloves petal dried, is ground into powder, weighs 1g in small beaker and add deionized water 10mL, It is added in autoclave, is put into 200 DEG C of baking oven pyroreaction 3 hours;
Cooling obtains brown solution after step 2, reaction terminate, and passes through centrifugation, 0.22 μm of filter filtering, then in 500- Dialysed 3 days in 1000D bag filters, it is pure carbon nano-particles solution to obtain brown color liquid;
Step 3, the carbon nano-particles solution vacuum freezedrying in step 2 obtained into brownish-yellow powder, that is, be purpose carbon Nano-particle, it is soluble in water to send blue-fluorescence;
Step 4, will the above-mentioned fluorescent carbon nano-particles aqueous solution be freeze-dried after obtain fluorescent carbon nano-particles, its relative quantity Sub- yield (using quinine sulfate as standard) is 10.9%.
Embodiment 5
Step 1, fresh cloves petal dried, is ground into powder, weighs 1g in small beaker and add deionized water 10ml, It is added in autoclave, is put into 200 DEG C of baking oven pyroreaction 5 hours;
Cooling obtains brown solution after step 2, reaction terminate, and passes through centrifugation, 0.22 μm of filter filtering, then in 500- Dialysed 3 days in 1000D bag filters, it is pure carbon nano-particles solution to obtain brown color liquid;
Step 3, the carbon nano-particles solution vacuum freezedrying in step 2 obtained into brownish-yellow powder, that is, be purpose carbon Nano-particle, it is soluble in water to send blue-fluorescence;
Step 4, will the above-mentioned fluorescent carbon nano-particles aqueous solution be freeze-dried after obtain fluorescent carbon nano-particles, its relative quantity Sub- yield (using quinine sulfate as standard) is 7.2%.
Embodiment 6
Step 1, fresh cloves petal dried, be ground into powder, weigh 1g in small beaker and add deionized water 10mL Then adding the stirring of 1g NaOH solids makes it fully dissolve, and is added in autoclave, is put into 200 DEG C of pyroreactions 4 of baking oven Hour;
Cooling obtains dark brown solution after step 2, reaction terminate, and passes through centrifugation, 0.22 μm of filter filtering, Ran Hou Dialysed 3 days in 500-1000D bag filters, it is pure carbon nano-particles solution to obtain brown liquid;
Step 3, the carbon nano-particles solution vacuum freezedrying in step 2 obtained into brown ceramic powder, i.e., received for purpose carbon Rice corpuscles, it is soluble in water to send green fluorescence;
Step 4, will the above-mentioned fluorescent carbon nano-particles aqueous solution be freeze-dried after obtain fluorescent carbon nano-particles, its relative quantity Sub- yield (using rhodamine 6G as standard) is 4.8%.
Embodiment 7
Step 1, fresh cloves petal dried, be ground into powder, weigh 1g in small beaker and add deionized water 10mL Then adding the stirring of 2g NaOH solids makes it fully dissolve, and is added in autoclave, is put into 200 DEG C of pyroreactions 4 of baking oven Hour;
Cooling obtains dark brown solution after step 2, reaction terminate, and passes through centrifugation, 0.22 μm of filter filtering, Ran Hou Dialysed 3 days in 500-1000D bag filters, it is pure carbon nano-particles solution to obtain brown liquid;
Step 3, the carbon nano-particles solution vacuum freezedrying in step 2 obtained into brown ceramic powder, i.e., received for purpose carbon Rice corpuscles, it is soluble in water to send green fluorescence;
Step 4, will the above-mentioned fluorescent carbon nano-particles aqueous solution be freeze-dried after obtain fluorescent carbon nano-particles, its relative quantity Sub- yield (using rhodamine 6G as standard) is 8.9%.
Embodiment 8
Step 1, fresh cloves petal dried, be ground into powder, weigh 1g in small beaker and add deionized water 10ml Then adding the stirring of 3g NaOH solids makes it fully dissolve, and is added in autoclave, is put into 200 DEG C of pyroreactions 4 of baking oven Hour;
Cooling obtains dark brown solution after step 2, reaction terminate, and passes through centrifugation, 0.22 μm of filter filtering, Ran Hou Dialysed 3 days in 500-1000D bag filters, it is pure carbon nano-particles solution to obtain brown liquid;
Step 3, the carbon nano-particles solution vacuum freezedrying in step 2 obtained into brown ceramic powder, i.e., received for purpose carbon Rice corpuscles, it is soluble in water to send green fluorescence;
Step 4, will the above-mentioned fluorescent carbon nano-particles aqueous solution be freeze-dried after obtain fluorescent carbon nano-particles, its relative quantity Sub- yield (using rhodamine 6G as standard) is 6.5%.
Embodiment 9
Pure carbon nano-particles obtained by embodiment 1-5 are subjected to fluorescence spectrum test, such as Figure 1A, B are embodiment 1-5 Fluorogram.Pure carbon nano-particles obtained by embodiment 6-8 are subjected to fluorescence spectrum test, such as Fig. 1 C are embodiment 6- 8 fluorescence spectra.
Embodiment 10
By blue-fluorescence quantum yield highest carbon nano-particles, i.e., the carbon nano-particles obtained in embodiment 2 carry out purple External spectrum is determined, and fluorescence excitation spectrum, emission spectra are determined, such as Fig. 2;By green fluorescence quantum yield highest carbon nano-particles, i.e., The carbon nano-particles obtained in embodiment 7 carry out ultraviolet spectroscopy, and fluorescence excitation spectrum, emission spectra are determined, such as Fig. 3.It will implement Fluorescent emission spectrogram of the carbon nano-particles solution under different excitation wavelengths in example 2 is measured, such as Fig. 4 A, in good transmitted wave Length belongs to blue light category in 450nm or so;By fluorescence of the carbon nano-particles solution under different excitation wavelengths in embodiment 2 Transmitting spectrogram is measured, such as Fig. 4 B, in good launch wavelength in 520nm or so, belongs to green glow category.
High-purity carbon nano-particles will be obtained in embodiment 2 and embodiment 7 and carry out infrared, TEM/HRTEM, XPS, XRD is characterized, Such as Fig. 5-8 obtains the high-purity carbon nano particle diameter respectively less than 10nm that the present invention is obtained, and the carbon nano-particles of blue light-emitting contain carboxylic Base, hydroxyl and amino groups, the carbon nano-particles of green light contain the groups such as carboxyl, hydroxyl, and two kinds of carbon nano-particles contain There is group to slightly have difference.
Embodiment 11
The fluorescent carbon nano-particles aqueous solution (2.8mg/mL) prepared by Example 2 is placed in fluorescence cuvette, is added respectively 17 kinds of common metal ion solutions (300mM), are sufficiently mixed uniform, scanning emission spectrum (the λ ex=in XRF 340nm, λ em=445nm), and the fluorescence intensity added after each ion is recorded, as shown in Figure 9 B, the carbon nanometer of embodiment 2 Particle is to Fe3+There are good selectivity, i.e. Fe3+The blue-fluorescence of the carbon nano-particles in embodiment 2 can be quenched.In order to Carbon nano-particles are calculated to Fe3+Detection range, Example 2 prepare the fluorescent carbon nano-particles aqueous solution (2.8mg/mL) put In fluorescence cuvette, the Fe of various concentrations is separately added into from low to high3+Solution, is sufficiently mixed uniformly, determines in various concentrations Fe3+The fluorescence of fluorescent carbon nano-particles in lower embodiment 2, such as Fig. 9 A are then drawn to Fe from figure3+Detection be limited to it is reachable 3.69×10-7Mol/L, detection range of linearity 0-150mol/L.And the fluorescent carbon nano-particles of the green light in embodiment 7 do not have There are good selection, such as Fig. 9 C to certain metal ion species.
Embodiment 12
The fluorescent carbon nano-particles aqueous solution (2.8mg/mL) prepared by Example 2 is placed in fluorescence cuvette, passes through profit Use various concentrations Fe3+C can be made in titration(Fe3+)With the linear relationship of fluorescence intensity, so as to determining in actual water sample (from In water) Fe3+Content, institute's measured value and the result that inductively coupled plasma spectrum generator (ICP) is determined be basically identical, sees Table 1, determining our method has reliability.
Embodiment 13
The carbon nano-particles (1.6mg/mL) of the green light prepared in embodiment 7 are placed in fluorescence cuvette, added not With its fluorescence is determined in pH solution (1.89-11.92), uniform, the scanning emission spectrum (λ in XRF is sufficiently mixed Ex=450nm, λ em=520nm), and record is added to the fluorescence intensity after each pH, as shown in Figure 10 A, in 1.89- Linear in the range of 8.95, i.e. pH is bigger, and fluorescence is stronger, and fluorescence is unaffected after 1.89 and 8.95 different repeated transformations, such as schemes 10B, illustrating the fluorescent carbon nano-particles of green light prepared by embodiment 7 has good sensitivity to pH.
Embodiment 14
The carbon nano-particles (1.6mg/mL) of the green light prepared in embodiment 7 are placed in fluorescence cuvette, added not With its fluorescence is determined in pH solution (1.89-8.95), the linear relationship of pH value of solution and fluorescence intensity is drawn, so as to determine PH in unknown real solution, institute's measured value and business pH analyzers measured value are very close to being shown in Table 2.
Embodiment 15
Different luminous carbon nano-particles in embodiment 2,7 are subjected to cytotoxicity test, various concentrations are prepared respectively Carbon nano-particles solution (0-50mg/mL) acts on human breast cancer cell line Bcap-37, i.e., carry out analyzing by conventional MTT experiment Go out the luminous carbon nano-particles of the difference prepared in embodiment 2,7 to cytotoxicity very little, such as Figure 11.
Embodiment 16
The carbon nano-particles aqueous solution (6mg/mL) of the transmitting blue-fluorescence prepared in embodiment 2 is used to mark people's mammary gland Cancer MCF-7 cells, such as Figure 12, Figure 12 A are that the carbon nano-particles aqueous solution (6mg/mL) only prepared in embodiment 2 is added to training Support in the DMEM nutrient solutions in MCF-7 cells, (excitation wavelength is 405nm to the laser confocal imaging after being incubated 10 minutes altogether, is connect The launch wavelength scope of receipts is 425-480nm), display blue-fluorescence is very strong;Figure 12 B-E are to add the carbon prepared in embodiment 2 The nano-particle aqueous solution (6mg/mL) is added in the DMEM nutrient solutions in culture MCF-7 cells, after being incubated 10 minutes altogether, immediately Add Fe3+(300mM) shows and elapsed over time, fluorescence gradually weakens in the laser confocal imaging of different time;Figure 12 F It is to add Fe3+In the intensity of cellular fluorescence figure of different time sections, show that the carbon nano-particles prepared in embodiment 2 can be in work Fe is detected in cell3+
Embodiment 17
The carbon nano-particles aqueous solution (5mg/mL) of the transmitting green fluorescence prepared in embodiment 7 is used to mark people's mammary gland Cancer MCF-7 cells, such as Figure 13 represents that the carbon nano-particles aqueous solution (5mg/mL) prepared in embodiment 7 is added to culture MCF-7 In DMEM nutrient solutions in cell, (excitation wavelength is 405nm, the transmitting of reception after being incubated altogether in different pH environment 10 minutes Wave-length coverage is 480-545nm) laser confocal imaging, it is very weak to be shown in the less sour environment green fluorescences of pH, and Neutrality and mild alkaline conditions green fluorescence larger pH is very strong, shows the carbon nano-particles of transmitting green fluorescence prepared by embodiment 7 Acid-base property can be detected in living cells.
Table 1 determines Fe in running water3+Content (n=3)
Table 2 determines unknown solution pH value
Embodiment above describes the preparation method and application of the present invention.The technical staff of the industry should know the present invention It is not restricted to the described embodiments, in the case where not departing from the scope of essence of the invention, various changes and modifications of the present invention are possible, this A little changes and improvements are each fallen within the scope of protection of the invention.

Claims (4)

1. a kind of controllable luminous carbon nano-particles, it is characterized in that being made up of following steps:
(1) fresh cloves petal is dried, is ground into powder, weighs 1-2g in small beaker and add deionized water 10mL, then It is fully dissolved by adding the stirring of 0-3gNaOH solids, be added in autoclave, be put into 150-250 DEG C of high temperature of baking oven Reaction 3-5 hours;
(2) cooling obtains brown or dark brown solution after reaction terminates, and passes through centrifugation, 0.22 μm of filter filtering, Ran Hou Dialysed 3 days in 500-1000D bag filters, it is pure carbon nano-particles solution to obtain brown color or brown liquid;
(3) the carbon nano-particles solution vacuum freezedrying in step (2) is obtained into brown color or brown ceramic powder, that is, is purpose carbon Nano-particle, it is soluble in water to send strong blueness or green fluorescence.
2. a kind of preparation method of controllable luminous carbon nano-particles described in claim 1, it is characterized in that comprising the following steps:
(1) fresh cloves petal is dried, is ground into powder, weighs 1-2g in small beaker and add deionized water 10mL, then It is fully dissolved by adding the stirring of 0-3g NaOH solids, be added in autoclave, be put into baking oven 150-250 DEG C high Temperature reaction 3-5 hours;
(2) cooling obtains brown or dark brown solution after reaction terminates, and passes through centrifugation, 0.22 μm of filter filtering, Ran Hou Dialysed 3 days in 500-1000D bag filters, it is pure carbon nano-particles solution to obtain brown color or brown liquid;
(3) the carbon nano-particles solution vacuum freezedrying in step (2) is obtained into brown color or brown ceramic powder, that is, is purpose carbon Nano-particle, it is soluble in water to send strong blueness or green fluorescence.
3. the application of controllable luminous carbon nano-particles described in claim 1, it is characterized in that being used to detect water-soluble as fluorescence probe Fe in liquid3+The pH value of concentration and the aqueous solution passes through the Fe in live cell fluorescent image checking living cells3+Concentration and work are thin PH value in born of the same parents.
4. the application of controllable luminous carbon nano-particles according to claim 3, it is characterized in that for detecting in the aqueous solution Fe3+Fe in concentration and living cells3+During concentration, the addition of NaOH solids in the step of lighting carbon nano-particles (1) is prepared For 0g;For detect the aqueous solution pH value and living cells pH value when, the NaOH in (1) the step of luminous carbon nano-particles are prepared The addition of solid is 1-3g.
CN201710482086.XA 2017-06-22 2017-06-22 A kind of controllable luminous carbon nano-particles and preparation method and application Active CN107151555B (en)

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CN108456519A (en) * 2018-07-06 2018-08-28 大连工业大学 A kind of N doping fluorescent carbon quantum dot and preparation method thereof
CN110055063A (en) * 2019-05-09 2019-07-26 山西大学 A kind of B, N, fluorescent orange carbon dots of S codope and its preparation method and application
CN112964683A (en) * 2021-02-08 2021-06-15 山西医科大学 Preparation method and application of folic acid modified nitrogen-doped graphene quantum dot/silver nano fluorescent probe

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Publication number Priority date Publication date Assignee Title
CN108456519A (en) * 2018-07-06 2018-08-28 大连工业大学 A kind of N doping fluorescent carbon quantum dot and preparation method thereof
CN110055063A (en) * 2019-05-09 2019-07-26 山西大学 A kind of B, N, fluorescent orange carbon dots of S codope and its preparation method and application
CN112964683A (en) * 2021-02-08 2021-06-15 山西医科大学 Preparation method and application of folic acid modified nitrogen-doped graphene quantum dot/silver nano fluorescent probe

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