CN107557002A - A kind of silica fluorescent carbon point nano-particle, preparation method and applications - Google Patents
A kind of silica fluorescent carbon point nano-particle, preparation method and applications Download PDFInfo
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- CN107557002A CN107557002A CN201710657422.XA CN201710657422A CN107557002A CN 107557002 A CN107557002 A CN 107557002A CN 201710657422 A CN201710657422 A CN 201710657422A CN 107557002 A CN107557002 A CN 107557002A
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Abstract
The invention belongs to field of nano material preparation, more particularly to a kind of preparation method and applications of silica fluorescent carbon point composite nanoparticle, the present invention is silicon source by carbon source, tetraethyl orthosilicate of glucose, and the adjustable silica fluorescent carbon point composite nanoparticle of fluorescence is prepared by copolycondensation under ethylenediamine catalysis.This method is easy to operate, reaction condition is gentle, by one-step method can fabricated in situ obtain silica fluorescent carbon point composite nanoparticle；And reaction yield is high, available for producing composite nanoparticle in enormous quantities.It is prepared that composite nanoparticle uniform particle diameter, regular appearance, photoluminescent property are stable, launch wavelength is adjustable and without exciting dependence.
Description
Technical field
The invention belongs to luminescent material and technical field of nano material, and in particular to a kind of silica-fluorescent carbon point is received
Rice corpuscles, preparation method and applications.
Background introduction
A kind of novel fluorescence carbon nanomaterial of the carbon point as rising in recent years, because glimmering with low toxicity, good biocompatibility
Photostability is strong, excites, resistance to photobleaching controllable with launch wavelength, no optical flare, is easy to extensive synthesis and functional modification
Etc. unrivaled advantage, turn into a new study hotspot in fluorescent nano material, all have in biology and field of medicaments wide
Wealthy application prospect.The fluorescence of carbon point has the characteristic that fluorescein or semiconductor-quantum-point do not possess, that is, right
Wavelength of fluorescence red shift with the increase of excitation wavelength of the dependence of excitation wavelength, i.e. carbon point.General carbon point is ultraviolet in 365nm
Under light irradiation, the fluorescence of blueness is sent.But because ultraviolet excitation is larger to biological bulk damage, and when carbon point is as fluorescence labeling
The blue-fluorescence sent is easily disturbed by impurity, greatly limit its bio-imaging application.So opened by the fluorescence for regulating and controlling carbon point
The longer novel fluorescence carbon point of launch wavelength is sent to be particularly important.
Nano particles of silicon dioxide be a kind of good biocompatibility, easy functionalization, nontoxic, size in tens nanometer to micro-
Meter level is controllable and constitutionally stable nano material.In nineteen sixty-eight, bySynthesize first.Hereafter, silica dioxide nano particle
The sub important application due in catalysis, detection and analysis and biomedicine field, and by extensive research.With titanium dioxide
Silicon nano is that basic architecture platform and the progress of carbon point are compound, by the restriction effect of silica, can regulate and control carbon point
Fluorescence and its dependent behavior is excited, had great importance to designing and developing multi-functional composite fluorescent nano particle.
The content of the invention
For in the prior art the defects of and deficiency, the present invention propose a kind of silica-fluorescent carbon point nano-particle,
Preparation method and applications, by controlling the addition of reacting middle catalyst can Effective Regulation silica-fluorescent carbon point nanometer
The fluorescence emission wavelengths of particle, the silica being prepared-fluorescent carbon point nano-particle can be applied to cell fluorescence imaging.
To reach above-mentioned purpose, the technical scheme that the present invention takes includes：
A kind of silica-fluorescent carbon point nano-particle, including silica nanometer silicon ball, in silica nanometer silicon ball
Have a fluorescent carbon point, the fluorescence emission peak of fluorescent carbon point is 550~518nm, the particle diameter of silica nanometer silicon ball for 110~
210nm。
Specifically, the preparing raw material of described silica-fluorescent carbon point nano-particle includes glucose and positive silicic acid second
Ester, preparation method are copolycondensation.
More specifically, the preparation of silica-fluorescent carbon point nano-particle is included using glucose as carbon source, tetraethyl orthosilicate
For silicon source, it is prepared under ethylenediamine catalysis by copolycondensation.
A kind of preparation method of silica-fluorescent carbon point nano-particle, including using glucose as carbon source, tetraethyl orthosilicate
For silicon source, it is prepared under ethylenediamine catalysis by copolycondensation.
Specifically, the amount ratio of carbon source and silicon source is 1g/3mL, the amount ratio of carbon source and ethylenediamine is 1g/0.2~2mL.
More specifically, glucose is mixed to get mixed solution with absolute ethyl alcohol and catalyst again after water dissolves, and mixing is molten
Liquid reacted at 40 DEG C 0.5h add tetraethyl orthosilicate continue react 3h, produce two after then being reacted 3 hours at 80 DEG C again
Silica-fluorescent carbon point nano-particle.
Described water and the amount ratio of absolute ethyl alcohol are 0.02~0.06.
Silica-fluorescent carbon point nano-particle described in any claim is used for the application of cell fluorescence imaging.
The titanium dioxide that the preparation method of silica-fluorescent carbon point nano-particle described in any claim is prepared
Silicon-fluorescent carbon point nano-particle is used for the application of cell fluorescence imaging.
Compared with prior art, advantages of the present invention includes：
(1) reaction condition of the present invention is gentle, operating procedure is simple, repeatability is high, realize one-step method prepare silica-
Fluorescent carbon point nano-particle；
(2) silica being prepared by the present invention-fluorescent carbon point nano-particle pattern rule, uniform particle diameter, with biography
The carbon point of system is compared, and has bright fluorescence, and its fluorescence emission peak can with catalyst ethylenediamine addition increase from
550nm is adjusted to 518nm；
(3) by the restriction effect of silica, the fluorescence of carbon point excites dependent behavior to be eliminated, and works as silica
It is etched after removing, this of carbon point excites dependence to recover again again.Silica-the fluorescent carbon point being prepared is received
Rice corpuscles can be applied to cell fluorescence imaging
Brief description of the drawings
Fig. 1 is the transmission electron microscope photo for silica-fluorescent carbon point nano-particle that embodiment 1 is prepared；
Fig. 2 is the fluorescent emission spectrogram for silica-fluorescent carbon point nano-particle that embodiment 1 is prepared；Insertion figure
For photo of the carbon point sample aqueous solution under 365nm ultraviolet lightings；
Fig. 3 is the laser confocal microscope (a) for silica-fluorescent carbon point nano-particle that embodiment 1 is prepared
Photograph via bright field and (b) details in a play not acted out on stage, but told through dialogues photo；
The present invention is illustrated below in conjunction with specification drawings and specific embodiments.
Embodiment
Following examples are that the present invention is further elaborated, for showing hair to the technical staff of association area and industry
The known preferred forms using the present invention of a person of good sense, but it is not intended to limit present disclosure and scope.Therefore, will in right
In the range of asking book and its equivalent, the present invention can be implemented by the mode different from the following specifically describes.
Embodiment 1：0.5g glucose is weighed first, is added 3mL deionized waters, is placed in ultrasonic dissolution in there-necked flask, treats Portugal
After grape sugar dissolving forms the solution of water white transparency, 50mL absolute ethyl alcohols and 0.1mL ethylenediamines are added.Then there-necked flask is placed in
In 40 DEG C of constant temperature oil baths, 200rpm mechanical agitations.After 0.5 hour, 1.5mL tetraethyl orthosilicates are added, continue stirring 3 hours.Instead
System is answered gradually to be changed into the emulsion of white from clear.Then, 80 DEG C of oil bath temperature is raised, keeps reaction solution backflow.3 is small
Shi Hou, reaction solution are changed into yellow by white.Carbon point/silica composite nanoparticle is centrifuged, and is washed with deionized water
Three times；It is 168nm to obtain particle diameter, and fluorescence emission wavelengths are 550nm silica-fluorescent carbon point nano-particle (see Fig. 1 and figure
2)。
Embodiment 2：0.5g glucose is weighed first, is added 3mL deionized waters, is placed in ultrasonic dissolution in there-necked flask, treats Portugal
After grape sugar dissolving forms the solution of water white transparency, 50mL absolute ethyl alcohols and 0.25mL ethylenediamines are added.Then there-necked flask is put
In 40 DEG C of constant temperature oil baths, 200rpm mechanical agitations.After 0.5 hour, 1.5mL tetraethyl orthosilicates are added, continue stirring 3 hours.
Reaction system is gradually changed into the emulsion of white from clear.Then, 80 DEG C of oil bath temperature is raised, keeps reaction solution backflow.3
After hour, reaction solution is changed into yellow by white.Silica-fluorescent carbon point nano-particle is centrifuged, and uses deionized water
Wash three times；It is 178nm to obtain particle diameter, and fluorescence emission wavelengths are 534nm silica-fluorescent carbon point nano-particle.
Embodiment 3：0.5g glucose is weighed first, is added 3mL deionized waters, is placed in ultrasonic dissolution in there-necked flask, treats Portugal
After grape sugar dissolving forms the solution of water white transparency, 50mL absolute ethyl alcohols and 1.0mL ethylenediamines are added.Then there-necked flask is placed in
In 40 DEG C of constant temperature oil baths, 200rpm mechanical agitations.After 0.5 hour, 1.5mL tetraethyl orthosilicates are added, continue stirring 3 hours.Instead
System is answered gradually to be changed into the emulsion of white from clear.Then, 80 DEG C of oil bath temperature is raised, keeps reaction solution backflow.3 is small
Shi Hou, reaction solution are changed into yellow by white.Silica-fluorescent carbon point nano-particle is centrifuged, and is washed with deionized water
Three times；It is 210nm to obtain particle diameter, and fluorescence emission wavelengths are 518nm silica-fluorescent carbon point nano-particle.
Embodiment 4：0.5g glucose is weighed first, is added 1mL deionized waters, is placed in ultrasonic dissolution in there-necked flask, treats Portugal
After grape sugar dissolving forms the solution of water white transparency, 50mL absolute ethyl alcohols and 0.25mL ethylenediamines are added.Then there-necked flask is put
In 40 DEG C of constant temperature oil baths, 200rpm mechanical agitations.After 0.5 hour, 1.5mL tetraethyl orthosilicates are added, continue stirring 3 hours.
Reaction system is gradually changed into the emulsion of white from clear.Then, 80 DEG C of oil bath temperature is raised, keeps reaction solution backflow.3
After hour, reaction solution is changed into yellow by white.Silica-fluorescent carbon point nano-particle is centrifuged, and uses deionized water
Wash three times；Obtain silica-fluorescent carbon point nano-particle that particle diameter is 110nm.
Embodiment 5：By human body cervical carcinoma cell (Hela cells) with 1 × 105The density of cells/well is inoculated into φ 35mm's
In Glass bottom culture dish, at 37 DEG C, contain 5%CO2Wet air atmosphere under cultivate；Treat that cell tight is adhered to culture wooden partition
Afterwards, nutrient solution is discarded, then, obtained silica-fluorescent carbon point in the example 1 that concentration is 50 μ g/mL is added toward in per hole
Nano-particle culture 4h, with the fresh repeated multiple times flushing cell of phosphate buffer solution.Utilize confocal laser scanning microscope
Silica-the fluorescence imaging ability of fluorescent carbon point nano-particle in the cell, excitation wavelength 405nm, sample collection it is glimmering
Optical wavelength range is 450-500nm, it was observed that green is presented in the HeLa cells of silica-fluorescent carbon point nanometer particle to mark
Fluorescence (see Fig. 3), the figure a in Fig. 3 represent photograph via bright field, and the figure b in Fig. 3 represents details in a play not acted out on stage, but told through dialogues photo, shows to prepare in embodiment one
Obtained silica-fluorescent carbon point nano-particle is imaged available for cell fluorescence.
Claims (9)
1. a kind of silica-fluorescent carbon point nano-particle, it is characterised in that including silica nanometer silicon ball, silica
There is fluorescent carbon point in nano silicon spheres, the fluorescence emission peak of fluorescent carbon point is 550~518nm, the particle diameter of silica nanometer silicon ball
For 110~210nm.
2. silica as claimed in claim 1-fluorescent carbon point nano-particle, it is characterised in that described silica-glimmering
The preparing raw material of light carbon point nano-particle includes glucose and tetraethyl orthosilicate, and preparation method is copolycondensation.
3. silica as claimed in claim 1-fluorescent carbon point nano-particle, it is characterised in that silica-fluorescent carbon point
The preparation of nano-particle is included using glucose as carbon source, and tetraethyl orthosilicate is silicon source, passes through copolycondensation system under ethylenediamine catalysis
It is standby to obtain.
A kind of 4. preparation method of silica-fluorescent carbon point nano-particle, it is characterised in that including using glucose as carbon source,
Tetraethyl orthosilicate is silicon source, is prepared under ethylenediamine catalysis by copolycondensation.
5. the preparation method of silica as claimed in claim 4-fluorescent carbon point nano-particle, it is characterised in that carbon source with
The amount ratio of silicon source is 1g/3mL, and the amount ratio of carbon source and ethylenediamine is 1g/0.2~2mL.
6. the preparation method of silica-fluorescent carbon point nano-particle as described in claim 4 or 5, it is characterised in that grape
Sugar is mixed to get mixed solution with absolute ethyl alcohol and catalyst again after water dissolves, and mixed solution reacts 0.5h at 40 DEG C and added again
Enter tetraethyl orthosilicate to continue to react 3h, silica-fluorescent carbon point nanoparticle is produced after then being reacted 3 hours under 80oC again
Son.
7. the preparation method of silica as claimed in claim 6-fluorescent carbon point nano-particle, it is characterised in that described
The amount ratio of water and absolute ethyl alcohol is 0.02~0.06.
8. silica-fluorescent carbon point nano-particle described in claim 1-3 any claims is imaged for cell fluorescence
Application.
9. the preparation method of silica-fluorescent carbon point nano-particle described in claim 4-7 any claims is prepared into
The silica arrived-fluorescent carbon point nano-particle is used for the application of cell fluorescence imaging.
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Cited By (6)
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| CN108048074A (en) * | 2018-01-15 | 2018-05-18 | 湖北大学 | A kind of hybrid inorganic-organic fluorescent nano particles for emitting glory and preparation method thereof |
| CN108949144A (en) * | 2018-08-27 | 2018-12-07 | 宝鸡文理学院 | A kind of Au@SiO2@CDs nanocomposite and preparation method thereof |
| CN110079303A (en) * | 2019-05-13 | 2019-08-02 | 吉林大学 | A kind of high stable without metallic silicon basal cell temperature phosphor material and preparation method thereof |
| CN112961669A (en) * | 2021-02-01 | 2021-06-15 | 苏州星烁纳米科技有限公司 | Preparation method of solid-phase carbon quantum dot, solid-phase carbon quantum dot prepared by same and light-emitting device |
| CN113480995A (en) * | 2021-08-04 | 2021-10-08 | 西北工业大学 | Nanoparticle-carbon dot @ silicon dioxide composite nanoparticle with long afterglow luminescence, long afterglow material and preparation method |
| CN113493197A (en) * | 2021-07-22 | 2021-10-12 | 哈尔滨工程大学 | Preparation method of carbon dot/porous silicon dioxide nanoenzyme with peroxidase-like activity |
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108048074A (en) * | 2018-01-15 | 2018-05-18 | 湖北大学 | A kind of hybrid inorganic-organic fluorescent nano particles for emitting glory and preparation method thereof |
| CN108949144A (en) * | 2018-08-27 | 2018-12-07 | 宝鸡文理学院 | A kind of Au@SiO2@CDs nanocomposite and preparation method thereof |
| CN110079303A (en) * | 2019-05-13 | 2019-08-02 | 吉林大学 | A kind of high stable without metallic silicon basal cell temperature phosphor material and preparation method thereof |
| CN110079303B (en) * | 2019-05-13 | 2021-07-06 | 吉林大学 | High-stability metal-silicon-free room temperature phosphorescent material and preparation method thereof |
| CN112961669A (en) * | 2021-02-01 | 2021-06-15 | 苏州星烁纳米科技有限公司 | Preparation method of solid-phase carbon quantum dot, solid-phase carbon quantum dot prepared by same and light-emitting device |
| CN113493197A (en) * | 2021-07-22 | 2021-10-12 | 哈尔滨工程大学 | Preparation method of carbon dot/porous silicon dioxide nanoenzyme with peroxidase-like activity |
| CN113493197B (en) * | 2021-07-22 | 2022-06-21 | 哈尔滨工程大学 | Preparation method of carbon dot/porous silica nanoenzyme with peroxidase-like activity |
| CN113480995A (en) * | 2021-08-04 | 2021-10-08 | 西北工业大学 | Nanoparticle-carbon dot @ silicon dioxide composite nanoparticle with long afterglow luminescence, long afterglow material and preparation method |
| CN113480995B (en) * | 2021-08-04 | 2022-07-22 | 西北工业大学 | Long-afterglow luminescent nanoparticle-carbon dot @ silicon dioxide composite nanoparticle, long-afterglow material and preparation method |
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