CN105969346B - A kind of method that microwave method prepares the fluorescence silicon quantum dot of fluorine doped - Google Patents
A kind of method that microwave method prepares the fluorescence silicon quantum dot of fluorine doped Download PDFInfo
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- CN105969346B CN105969346B CN201610354100.3A CN201610354100A CN105969346B CN 105969346 B CN105969346 B CN 105969346B CN 201610354100 A CN201610354100 A CN 201610354100A CN 105969346 B CN105969346 B CN 105969346B
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Abstract
A kind of method that the fluorescence silicon quantum dot of fluorine doped is prepared the invention discloses microwave method, its step are：1) mass fraction is prepared as 4% 5% sodium citrate aqueous solution, adds silane coupling agent into sodium citrate aqueous solution, and the mass ratio of silane coupling agent and sodium citrate aqueous solution is 10 30：80, after mixing, add the ethanol solution of the tert-butyl alcohol containing perfluor, the molar ratio of the perfluor tert-butyl alcohol and silane coupling agent is 1：5 15, the volume ratio of absolute ethyl alcohol and water is 1：5 10, ultrasonic disperse is uniform, obtains reaction precursor；2) reaction precursor is transferred in reaction tube, microwave heats reaction tube to after 160 180 DEG C, reacts 15 30 minutes, and the system that will react gained is cooled to room temperature, and obtains yellow solution；3) yellow solution is dialysed and removes impurity, then with filtering with microporous membrane, finally freezed filtrate.This method only needs simple one-step synthesis, and fluorescence intensity height, uniform particle diameter, the fluorescence silicon quantum dot of the surface fluorine doped of good dispersion is just made.
Description
Technical field
The invention belongs to silicon quantum dot prepare and19F nmr imaging techniques field, and in particular to prepared by a kind of microwave method
The method of the fluorescence silicon quantum dot of fluorine doped.
Background technology
Quantum dot is a kind of nano material of quasi-zero dimension, is made of a small amount of atom, diameter is between 1-10nm.Due to by
To the influence of quantum confined effect, quantum dot is with fluorescence intensity is high, Stokes shift is big, exciting light spectrum width, launch wavelength
By unique optical properties such as size regulation and control.But traditional semiconductor-quantum-point such as II-VI group quantum dot (CdX, X=Se, S,
Te) since containing heavy metal element such as Cd, its physiological-toxicity limits development of such quantum dot in field of biology.And silicon amount
Son point is due to good biocompatibility and nontoxicity, and unique optical property and high surface-active, silicon quantum
Point achieves more and more applications as fluorescence probe in optical imagery, oncotherapy etc..
Magnetic resonance imaging (MRI) technology is a kind of common at this stage without invasive early diagnosis of tumor method, tradition
's1H MRI strengthen usually using contrast agent1The signal contrast of H, but since there are a large amount of H in human body2O and it is some other in
The background signal of source property material so that1H MRI signal-to-noise ratio is low.In order to solve this problem, heteronuclear MRI is (such as13C,23Na,31P
,19F) technology has obtained more and more development.Wherein,19F has 100% natural abundance, spin quantum number 1/2, magnetic rotation
Than being for 40.08MHz/T, its NMR sensitivity1The 83% of H, in addition,19The chemical shift span scope of F it is wide (>
350ppm), and19F is existed only in bone and tooth, this solid-state form cause its T2 relaxation times very it is short cause it is extremely low
Background signal is without being detected, that is to say, that19F disturbs almost without background signal in vivo, therefore19F MRI are in life
There is great application potential in the research of thing molecular imaging.
In conclusion with reference to silicon quantum dot uniqueness optical property and19The high sensitivity of F MRI, prepares a kind of fluorine doped
Fluorescence silicon quantum dot can be used as the detection unit of difunctional (fluorescence and nuclear-magnetism), and there is greatly application to dive in molecular imaging
Power.
The content of the invention
To solve the above-mentioned problems of the prior art, the present invention provides the fluorescence silicon amount that a kind of microwave method prepares fluorine doped
The method of son point, this method use microwave attenuation materials method, only need simple one-step synthesis, it is possible to fluorescence intensity is made
Height, uniform particle diameter, the fluorescence silicon quantum dot of the surface fluorine doped of good dispersion.
Technical solution is used by realizing above-mentioned purpose of the present invention：
A kind of method that microwave method prepares the fluorescence silicon quantum dot of fluorine doped, includes the following steps：
1) trisodium citrate dihydrate is dissolved in ultra-pure water, prepares the sodium citrate aqueous solution that mass fraction is 4%-5%,
Add silane coupling agent into sodium citrate aqueous solution, the mass ratio of silane coupling agent and sodium citrate aqueous solution is 10-30：
80, after mixing, add the ethanol solution of the tert-butyl alcohol containing perfluor, the molar ratio of the perfluor tert-butyl alcohol and silane coupling agent is
1：The volume ratio of 5-15, absolute ethyl alcohol and water is 1:5-10, ultrasonic disperse is uniform, obtains the precursors of water white transparency；
2) precursors are transferred in reaction tube, microwave heats reaction tube to after 160-180 DEG C, 15-30 points of reaction
The system for reacting gained, is cooled to room temperature by clock after the completion of reaction, obtains the yellow solution of clarification shape；
3) yellow solution bag filter is dialysed in ultra-pure water and removes impurity, the solution that gained is completed in dialysis is filtered with micropore
Membrane filtration, filtrate is freezed, up to the fluorescence silicon quantum dot of fluorine doped.
The silane coupling agent is 3- aminopropyl trimethoxysilanes or 3- aminopropyl triethoxysilanes.
In step 1), the mass fraction of sodium citrate aqueous solution is 4.65%, silane coupling agent and sodium citrate aqueous solution
Mass ratio be 1：4, the molar ratio of the perfluor tert-butyl alcohol and silane coupling agent is 1:5, the volume ratio of absolute ethyl alcohol and water is 1:6.
In step 3), the molecular cut off of bag filter is 500Da or 1000Da.
In step 3), dialyse 4-6 times, when the time dialysed every time is 2-4 small, when total dialysis time is small no more than 24.
In step 3), the aperture of miillpore filter is 220nm.
Compared with prior art, the advantages of the present invention are：
This method prepares the fluorescence silicon quantum dot of fluorine doped using a step microwave attenuation materials method, and preparation process is simple, reaction
Time is short, easily-controlled reaction conditions, and fluorescence silicon quantum dot fluorescence intensity height, uniform particle diameter, the good dispersion of obtained fluorine doped
And it can show stronger19F-NMR signals, make its bio-sensing, fluorescence imaging and19Valency is applied with important in F-MRI fields
Value.
Brief description of the drawings
Fig. 1 is the transmission electron microscope picture of the fluorescence silicon quantum dot of fluorine doped made from embodiment 1.
Fig. 2 is the high-resolution-ration transmission electric-lens figure of the fluorescence silicon quantum dot individual particle of fluorine doped made from embodiment 1.
Fig. 3 is the dynamic light scattering diagram of the fluorescence silicon quantum dot of fluorine doped made from embodiment 1.
Fig. 4 is the UV absorption and fluorescence emission spectrogram of compound of the fluorescence silicon quantum dot of fluorine doped made from embodiment 1.
Fig. 5 is the fluorescence silicon quantum dot of fluorine doped made from embodiment 1 in x-ray photoelectron spectroscopy figure.
Fig. 6 is the fluorine spectrogram of the fluorescence silicon quantum dot of fluorine doped made from embodiment 1.
Fig. 7 is the dynamic light scattering diagram of the fluorescence silicon quantum dot of fluorine doped made from embodiment 2.
Fig. 8 is the UV absorption and fluorescence emission spectrogram of compound of the fluorescence silicon quantum dot of fluorine doped made from embodiment 2.
Fig. 9 is the dynamic light scattering diagram of the fluorescence silicon quantum dot of fluorine doped made from embodiment 3.
Figure 10 is the UV absorption and fluorescence emission spectrogram of compound of the fluorescence silicon quantum dot of fluorine doped made from embodiment 3.
Embodiment
With reference to specific embodiment, the present invention is described in detail.
Embodiment 1
1) 139mg trisodium citrate dihydrates are dissolved in 3ml ultra-pure waters, prepare the sodium citrate that mass fraction is 4.65%
Solution, 750ul 3- aminopropyl trimethoxysilanes are added into sodium citrate solution, after mixing, are added 0.5ml and are contained 120
The ethanol solution of the ul perfluor tert-butyl alcohols, ultrasonic 2-5min make it be uniformly dispersed, and obtain the precursors of water white transparency.
2) precursors are transferred in reaction tube, microwave heats reaction tube to after 170 DEG C, reacting 15min, reaction
After the completion of will react gained system be cooled to room temperature (20-30 DEG C), obtain the yellow solution of clarification shape, which exists
Strong blue-fluorescence is shown under 365nm ultra violet lamps, and there is good water dispersible.
3) yellow solution is dialysed with the bag filter of molecular cut off 1000Da in ultra-pure water and removes unreacted salt etc.
Impurity, dialyses 5 times, and the volume of ultra-pure water used in dialysis is 3L every time, and when each dialysis time is 4 small, gained is completed in dialysis
The filtering with microporous membrane of solution 220nm, filtrate is freezed, and up to the fluorescence silicon quantum dot of fluorine doped, is labeled as19F-SiQDs, will
The fluorescence silicon quantum dot of the fluorine doped of gained is redissolved in ultra-pure water, and the fluorescence silicon quantum dot for being configured to certain density fluorine doped is molten
Liquid, every property of the fluorescence silicon quantum dot for detecting the fluorine doped.
Will be manufactured in the present embodiment19F-SiQDs is scanned with transmission electron microscope, the transmission electron microscope picture of gained as shown in Figure 1,
It is from figure 1 it appears that manufactured in the present embodiment19F-SiQDs good dispersions, uniform particle diameter, average grain diameter 4.43nm.
Will be manufactured in the present embodiment19F-SiQDs is scanned with high resolution TEM, the height of the individual particle of gained
Resolved transmittance electron microscope from Fig. 2 as shown in the figure, can substantially observe19The lattice structure of F-SiQDs, upper right corner illustration are pair
The electronics selected diffraction collection of illustrative plates answered, measures19The spacing of lattice of F-SiQDs is 0.19nm, is (220) crystal face.
Will be manufactured in the present embodiment19F-SiQDs carries out dynamic light scattering detection, dynamic light scattering diagram such as Fig. 3 institutes of gained
Show, from figure 3, it can be seen that19The average hydration particle diameter of F-SiQDs is 6.11nm.
Will be manufactured in the present embodiment19F-SiQDs carries out UV absorption and fluorescence emission spectrum detection, the UV absorption of gained
Spectrogram as shown in figure 4, figure 4, it is seen that19The uv-absorption maximum wavelength of F-SiQDs is 350nm, emission maximum ripple
A length of 450nm.
Will be manufactured in the present embodiment19F-SiQDs carries out x-ray photoelectron spectroscopy detection, the x-ray photoelectron spectroscopy of gained
As shown in figure 5, from figure 5 it can be seen that19There are C (C in F-SiQDs1SWith reference to can be 284.8eV), N (N1SWith reference to can be
399.07eV)、O(O1SWith reference to can be 531.87eV), Si (Si2pWith reference to can be 102.26eV) and F (F1SWith reference to can be
688.13eV) element.
Will be manufactured in the present embodiment19F-SiQDs (the fluorescence silicon quantum dot solution for being configured to the fluorine doped of 20mg/ml) carries out fluorine
Spectrum detection, gained fluorine spectrum as shown in fig. 6, it can be seen from figure 7 that19F-NMR signals be it is one unimodal, chemical shift-
75.34ppm。
Embodiment 2
1) 139mg trisodium citrate dihydrates are dissolved in 3ml ultra-pure waters, prepare the sodium citrate that mass fraction is 4.65%
Solution, 750ul 3- aminopropyl trimethoxysilanes are added into sodium citrate solution, after mixing, are added 0.5ml and are contained 60
The ethanol solution of the ul perfluor tert-butyl alcohols, ultrasonic 2-5min make it be uniformly dispersed, and obtain the precursors of water white transparency.
2) precursors are transferred in reaction tube, microwave heats reaction tube to after 170 DEG C, reacting 15min, reaction
After the completion of will react gained system be cooled to room temperature (20-30 DEG C), obtain the yellow solution of clarification shape, which exists
Strong blue-fluorescence is shown under 365nm ultra violet lamps, and there is good water dispersible.
3) yellow solution is dialysed with the bag filter of molecular cut off 1000Da in ultra-pure water and removes unreacted salt etc.
Impurity, dialyses 5 times, and the volume of ultra-pure water used in dialysis is 3L every time, and when each dialysis time is 3 small, gained is completed in dialysis
The filtering with microporous membrane of solution 220nm, filtrate is freezed, and up to the fluorescence silicon quantum dot of fluorine doped, is labeled as19F-SiQDs, will
The fluorescence silicon quantum dot of the fluorine doped of gained is redissolved in ultra-pure water, and the fluorescence silicon quantum dot for being configured to certain density fluorine doped is molten
Liquid, every property of the fluorescence silicon quantum dot for detecting the fluorine doped.
Will be manufactured in the present embodiment19F-SiQDs carries out dynamic light scattering detection, dynamic light scattering diagram such as Fig. 7 institutes of gained
Show, from figure 7 it can be seen that19The average hydration particle diameter of F-SiQDs is 5.38nm.
Will be manufactured in the present embodiment19F-SiQDs carries out UV absorption and fluorescence emission spectrum detection, the UV absorption of gained
With fluorescence emission spectrogram of compound as shown in figure 8, from figure 8, it is seen that the uv-absorption maximum wavelength for measuring 19F-SiQDs is
350nm, maximum emission wavelength 450nm.
Embodiment 3
1) 139mg trisodium citrate dihydrates are dissolved in 3ml ultra-pure waters, prepare the sodium citrate that mass fraction is 4.65%
Solution, 750ul 3- aminopropyl trimethoxysilanes are added into sodium citrate solution, after mixing, are added 0.5ml and are contained 400
The ethanol solution of the ul perfluor tert-butyl alcohols, ultrasonic 2-5min make it be uniformly dispersed, and obtain the precursors of water white transparency.
2) precursors are transferred in reaction tube, microwave heats reaction tube to after 170 DEG C, reacting 15min, reaction
After the completion of will react gained system be cooled to room temperature (20-30 DEG C), obtain the yellow solution of clarification shape, which exists
Strong blue-fluorescence is shown under 365nm ultra violet lamps, and there is good water dispersible.
3) yellow solution is dialysed with the bag filter of molecular cut off 1000Da in ultra-pure water and removes unreacted salt etc.
Impurity, dialyses 5 times, and the volume of ultra-pure water used in dialysis is 3L every time, and when each dialysis time is 3 small, gained is completed in dialysis
The filtering with microporous membrane of solution 220nm, filtrate is freezed, and up to the fluorescence silicon quantum dot of fluorine doped, is labeled as19F-SiQDs, will
The fluorescence silicon quantum dot of the fluorine doped of gained is redissolved in ultra-pure water, and the fluorescence silicon quantum dot for being configured to certain density fluorine doped is molten
Liquid, every property of the fluorescence silicon quantum dot for detecting the fluorine doped.
Will be manufactured in the present embodiment19F-SiQDs carries out dynamic light scattering detection, dynamic light scattering diagram such as Fig. 9 institutes of gained
Show, as seen from Figure 9,19The average hydration particle diameter of F-SiQDs is 4.30nm.
Will be manufactured in the present embodiment19F-SiQDs carries out UV absorption and fluorescence emission spectrum detection, the UV absorption of gained
It is as shown in Figure 10 with fluorescence emission spectrogram of compound, from fig. 10 it can be seen that the uv-absorption maximum wavelength for measuring 19F-SiQDs is
350nm, maximum emission wavelength 450nm.
Claims (6)
1. a kind of method that microwave method prepares the fluorescence silicon quantum dot of fluorine doped, it is characterised in that include the following steps：
1) trisodium citrate dihydrate is dissolved in ultra-pure water, prepares the sodium citrate aqueous solution that mass fraction is 4%-5%, Xiang Ning
Add silane coupling agent in lemon acid sodium aqueous solution, the mass ratio of silane coupling agent and sodium citrate aqueous solution is 10-30：80, mix
After closing uniformly, the ethanol solution of the tert-butyl alcohol containing perfluor is added, the molar ratio of the perfluor tert-butyl alcohol and silane coupling agent is 1：5-
15, the volume ratio of absolute ethyl alcohol and water is 1:5-10, ultrasonic disperse is uniform, obtains the precursors of water white transparency；
2) precursors being transferred in reaction tube, microwave heats reaction tube to after 160-180 DEG C, reacts 15-30 minutes,
The system for reacting gained is cooled to room temperature after the completion of reaction, obtains the yellow solution of clarification shape；
3) yellow solution bag filter is dialysed in ultra-pure water and removes impurity, the solution miillpore filter mistake of gained is completed in dialysis
Filter, filtrate is freezed, up to the fluorescence silicon quantum dot of fluorine doped.
2. the method that microwave method according to claim 1 prepares the fluorescence silicon quantum dot of fluorine doped, it is characterised in that：Described
Silane coupling agent is 3- aminopropyl trimethoxysilanes or 3- aminopropyl triethoxysilanes.
3. the method that microwave method according to claim 1 prepares the fluorescence silicon quantum dot of fluorine doped, it is characterised in that：Step 1)
In, the mass fraction of sodium citrate aqueous solution is 4.65%, and the mass ratio of silane coupling agent and sodium citrate aqueous solution is 1：4,
The molar ratio of the perfluor tert-butyl alcohol and silane coupling agent is 1:5, the volume ratio of absolute ethyl alcohol and water is 1:6.
4. the method that microwave method according to claim 1 prepares the fluorescence silicon quantum dot of fluorine doped, it is characterised in that：Step 3)
In, the molecular cut off of bag filter is 500Da or 1000Da.
5. the method that microwave method according to claim 1 prepares the fluorescence silicon quantum dot of fluorine doped, it is characterised in that：Step 3)
In, dialyse 4-6 times, when the time dialysed every time is 2-4 small, when total dialysis time is small no more than 24.
6. the method that microwave method according to claim 1 prepares the fluorescence silicon quantum dot of fluorine doped, it is characterised in that：Step 3)
In, the aperture of miillpore filter is 220nm.
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| CN111573679B (en) * | 2020-05-08 | 2022-06-21 | 江苏大学 | Method for preparing water-soluble fluorescent silicon quantum dots by microwave method |
| CN114214062A (en) * | 2021-12-23 | 2022-03-22 | 郑州中科生物医学工程技术研究院 | Preparation method of fluorine-doped silicon quantum dots and application of fluorine-doped silicon quantum dots in detection of carmine |
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Effective date of registration: 20210223 Address after: 430071 Xiao Hong, Wuchang District, Wuhan District, Hubei, Shanxi, 30 Patentee after: Institute of precision measurement science and technology innovation, Chinese Academy of Sciences Address before: 430071 No.30, Xiaohongshan West District, Wuhan City, Hubei Province Patentee before: WUHAN INSTITUTE OF PHYSICS AND MATHEMATICS, CHINESE ACADEMY OF SCIENCES |
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Application publication date: 20160928 Assignee: Wuhan Lianying Life Science Instrument Co.,Ltd. Assignor: Institute of precision measurement science and technology innovation, Chinese Academy of Sciences Contract record no.: X2021980001566 Denomination of invention: A microwave method for preparing fluorine doped fluorescent silicon quantum dots Granted publication date: 20180508 License type: Common License Record date: 20210310 |