CN106519098B - A kind of preparation method of core-shell quanta dots/polystyrene fluorescent microsphere - Google Patents
A kind of preparation method of core-shell quanta dots/polystyrene fluorescent microsphere Download PDFInfo
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Abstract
The present invention relates to nano-functional material design fields, disclose a kind of preparation method of core-shell quanta dots/polystyrene fluorescent microsphere, successfully a large amount of quantum dots are coated in polystyrene microsphere using emulsion polymerization, it remains the major advantage of investment and overcomes it and coat unevenly, the problems such as covering amount is inadequate, quantum dot leaks outside disadvantage, the high quantum dot fluorescence microballoon of uniform particle sizes, fluorescent stabilization, fluorescence intensity is prepared, synthetic method of the present invention is simple, microspherulite diameter is controllable, it is reproducible, biomolecule detection can be used in.
Description
Technical field
The present invention relates to nano-functional material design field, especially a kind of core-shell quanta dots/polystyrene fluorescent microsphere
Preparation method, quantum dot/polystyrene fluorescent microsphere of synthesis can be used for highly sensitive bioanalysis and detection.
Background technique
Fluorescent microsphere refers to that fluorescent material passes through investment, physisorphtion, self-assembly method, chemical bonding, copolymerization method
The methods of absorption or be coated on the inside of microballoon and the nanometer that is formed to micron order load fluorescent material microballoon.Outside microballoon
Shape is generally spherical shape, so referred to as fluorescent microsphere, fluorescent microsphere morphosis is stable, has protective effect and table to fluorescent material
Face modifiability possesses great potential in the fields such as label, detection, tracer, immune medicine, high-flux medicaments sifting.
Quantum dot is the size of three dimensions all at 100 nanometers hereinafter, radius is less than or close to laser Bohr radius, energy
Enough receive a kind of semiconductor nanoparticle that laser generates fluorescence.Novel semi-conductor luminescent material has wide absorption peak, narrow
And symmetrical emission peak, and emission peak, that is, luminescent color is with size adjustable and higher fluorescence intensity, stronger anti-light bleaching
The features such as ability, can overcome the fluorescence signal of conventional fluorescent material is unstable, preparation condition is harsh, prompt fluorescence interference etc. ask
Topic has more superior performance compared with conventional organic dyes, is a kind of fluorescence probe prepared product of great potential.Its application neck
Domain is more and more extensive, especially its potential application value in the research such as immuno-biology and Clinical laboratory medicine, oneself causes
The very big concern of numerous scientific workers, luminescent quantum dot mark large biological molecule as fluorescent reagent probe, exactly in recent years
Come the nano material that rapidly develops field of bioanalysis one of important application.
Polystyrene is that the fluorescent microsphere of carrier is one of most common microballoon, and polystyrene microsphere is due to specific surface area
Greatly, the advantages that functional group and functional group reactions are strong is easily modified on uniform particle sizes, surface, is ideal fluorescent material carrier,
Polystyrene microsphere can be downloaded on polystyrene microsphere as carrier, quantum dot by swelling, absorption, investment fashion, still
These preparation methods all have the shortcomings that some or it is some fatal, cause these microballoons that can not be mass produced and be commercialized；Such as
The fluorescent microsphere long-time quantum dot of swelling method preparation is easy to be left out；The fluorescent microsphere of physical absorption preparation is easy by the external world
The influence of environment, such as solvent, acid, alkali be easy to cause the omitted and fluorescent quenching of absorption quantum dot.Although common investment
Synthesis condition is slightly harsh, and there are also advantages, is such as formed the inside that quantum dot is coated on microballoon by monomer polymerization mode
Stable quantum dot fluorescence microballoon, greatly reduces the influence of external environment, greatly improves the stability of quantum dot fluorescence microballoon,
And can be coupled by surface modification functional group with biomolecule, for highly sensitive bioanalysis and detection, but by more
Year development is remained on there are cladding in quantum dot/polystyrene microsphere of investment preparation is uneven, covering amount not enough, quantum dot
Leakage, the problems such as microspherulite diameter is big.
Summary of the invention
The purpose of the present invention is to provide a kind of core-shell quanta dots/polystyrene fluorescent microsphere preparation methods, using cream
Liquid, which polymerize, is successfully coated on a large amount of quantum dots in polystyrene microsphere, remains the major advantage of investment and overcomes it and wraps
Cover it is uneven, covering amount not enough, quantum dot leakage the problems such as disadvantage, prepared uniform particle sizes, fluorescent stabilization, fluorescence intensity pole
High quantum dot fluorescence microballoon, synthetic method of the present invention is simple, microspherulite diameter is controllable, reproducible, can be used in biomolecule and examine
It surveys.
To realize above-mentioned technical purpose and the technique effect, the invention discloses a kind of core-shell quanta dots/polyphenyl second
The preparation method of alkene fluorescent microsphere, core-shell quanta dots are prepared using thermal cycle coupled method, and are clicked through again to quantum using mercaptan
Quantum dot is embedded in polystyrene microsphere by row surface modification using emulsion polymerization, and it is glimmering to obtain core-shell quanta dots/polystyrene
Light microballoon, it is specific the preparation method is as follows:
Step 1: weighing surfactant 2-20 parts, 0.2-2 parts of sodium bicarbonate, 2-30 parts of dispersing agent, be added to vial
It is interior, it adds deionized water ultrasound 5-10 minutes, forms uniform mixed aqueous solution A, using 100 parts of styrene as reference standard；
Step 2: core-shell quanta dots 10-150 parts is weighed, 100 parts of styrene and 4-30 parts of tert-butyl acrylates are added,
Ultrasound 5 minutes, form uniform oil phase liquid B in ice bath；
Step 3: magnetic agitation 10 minutes after both water solution A and oil phase liquid B are mixed, then ultrasound 5-20 points in ice bath
Clock forms stable microemulsion；
Step 4: microemulsion being transferred in there-necked flask, leads to the oxygen in 30 minutes removal there-necked flasks of nitrogen, is warming up to 60-
80 DEG C, it is added initiator 1-30 parts, under magnetic stirring, is reacted 6-12 hours, by product centrifugal purification, it is glimmering to obtain polystyrene
Light microballoon.
Wherein, by thermal cycle coupled method, the epitaxially grown quantum dot shell on quantum dot core is 1-16 to core-shell quanta dots
Layer, the fluorescence spectra emission wavelength of core-shell quanta dots are 548nm-750nm.
Wherein, the mercaptan ligand of core-shell quanta dots surface modification is alkyl hydrosulfide, core-shell quanta dots ligand exchange amount used
Son point and the mass ratio of alkyl hydrosulfide are 1:(0.5-2).
Wherein, surfactant is dodecyl sulphate amine, lauryl sodium sulfate, dodecyl sodium sulfate in step 1
Or one of dodecyl ethyoxyl sulfobetaines, dispersing agent are the polyvinylpyrrolidone of each molecular weight.
Wherein, initiator is one of potassium peroxydisulfate or ammonium persulfate in step 4.
The invention has the following advantages:
1. the present invention by the ligand exchange of quantum dot, the microemulsion of inorganic salts, ester is added, synthesized uniform particle sizes,
The high quantum dot fluorescence microballoon of fluorescent stabilization, fluorescence intensity, can be used for highly sensitive bioanalysis by subsequent modified with functional group
And fluorescence immune chromatography quickly detects.
2. the fluorescence of conventional fluorescent material can be overcome by using quantum dot fluorescence microballoon compared with conventional fluorescent microballoon
The problems such as jitter, preparation condition are harsh, prompt fluorescence interferes.
3. quantum dot is successfully embedded in polystyrene microsphere, relative to swelling method, physisorphtion etc., stability is more
Good, quantum dot will not be left out out of microballoon, while resistance to harshness physiological condition effect is more preferable under the protection of microballoon.
Detailed description of the invention
Fig. 1 is flow diagram of the invention.
Fig. 2 is different shell thickness core-shell quanta dots fluorescent emission figures of the invention.
Fig. 3 is different shell thickness core-shell quanta dots fluorescence quantum yield figures and fluorescent emission peak width of the invention
Figure.
Fig. 4 is different shell thickness core-shell quanta dots transmission electron microscope pictures of the invention.
Fig. 5 is core-shell quanta dots of the invention/polystyrene fluorescent microsphere fluorescence emission spectrum.
Fig. 6 is that different polystyrene dosages of the invention synthesize fluorescent microsphere transmission electron microscope picture.
Specific embodiment
In order to make the objectives, technical solutions, and advantages of the present invention clearer, with reference to the accompanying drawings and embodiments, right
The present invention is further elaborated.
Embodiment 1
The invention discloses a kind of core-shell quanta dots/polystyrene fluorescent microsphere preparation method, wherein core-shell quanta dots
By taking zincblende CdSe/CdS quantum dot as an example, but it is not limited to this kind of quantum dot.
The synthesis and purification of zinc blende-type CdSe quantum dot: the Cd (St) of 0.2712g is weighed2In three-necked flask, then move
Enter the octadecenic acid of 7mL；It is stirred at room temperature, vacuumizes, lead to nitrogen, then increase temperature to 100 DEG C, to promote to melt, and after
It continuous logical nitrogen 10 minutes, is rapidly heated, when system temperature is raised to 250 DEG C, the Se- octadecenic acid for being rapidly injected 2mL 0.1M is outstanding
Turbid re-injects the Se- octadecenic acid suspension of 0.05mL 0.1M after keeping this temperature to carry out reaction 8 minutes, and 3-4 minutes
Afterwards, third time injects the Se- octadecenic acid suspension of 0.05mL 0.1M.Hereafter 3-4 minutes every, re-inject the Se- ten of 0.1M
Eight olefin(e) acid suspensions reach desired size until the size of quantum dot；During reacting progress, it can be drawn with syringe a small amount of molten
Liquid measures spectrum in cuvette, through UV-Vis to monitor extent of reaction.When the nanocrystal of reaction acquisition desired size, i.e.,
It carves and stops heating, when reaction solution is quickly cooled to 50 DEG C, carry out in-situ purification.
After purification by the CdSe core of preparation, it measures fluorescence or ultraviolet-visible absorption measures absorbance, pass through delustring system
The amount of the quantitative CdSe core substance for being 3.0nm for the partial size of measurement of number is 2*10-7The system of mol, coats 6 layers of shell, and every layer
The Cd(DDTC for the 0.1mol/L that shell needs to be added)2Single precursor volume is respectively 0.1,0.16,0.23,0.31,0.385 He
0.48mL。
The 1mL CdSe solution for taking 2mL dodecane, 3mL oleyl amine and in-situ purification to cross is added in there-necked flask.Logical nitrogen 10
Minute, it is warming up to 80 DEG C；The shell precursor for injecting corresponding amount, in the 1st layer of injection precursor, solution temperature is set as 80 DEG C, preceding
Liquid solution is driven to be injected into there-necked flask with syringe.It is maintained 10 minutes at 80 DEG C, then heats to 160 DEG C, divided in holding 20
Stop heating after clock, reaction solution is made to be cooled to 80 DEG C, the growth pattern of the 2nd layer to the 6th layer shell is with the 1st layer, only
Growth temperature is changed to 150 DEG C.Complete the epitaxial growth of shell.
The ligand exchange of CdSe/CdS quantum dot:
The ligand exchange of CdSe/CdS, which is comprised the concrete steps that, is dissolved in 8mL first for 0.12g CdSe/CdS quantum dot after purification
In benzene, 0.8g lauryl mercaptan is added.It is transferred in 50mL single port bottle, is warming up to 75 DEG C.Heat preservation 5 hours.Acetone is added
Precipitating, 5000rmp centrifugation.
The synthesis of core-shell quanta dots/polystyrene fluorescent microsphere:
The synthesis of polystyrene fluorescent microsphere: 0.017g lauryl sodium sulfate, 0.005g sodium bicarbonate, 0.02g are weighed
Polyvinylpyrrolidone is added in 50mL vial, adds 15mL deionized water ultrasound 5 minutes, formation uniformly mixes water-soluble
Liquid.The 0.04g CdSe/CdS quantum dot for weighing dodecyl sulphur ligand, adds 0.5mL styrene and the tertiary fourth of 100L acrylic acid
Ester.Ultrasound 5 minutes, form uniform oil phase liquid in ice bath.Magnetic agitation 10 minutes after the two is mixed, then surpass in ice bath
Sound 10 minutes, form stable microemulsion.Microemulsion is transferred in 100mL there-necked flask, 20 minutes removal there-necked flasks of nitrogen are led to
In oxygen.It is warming up to 75 DEG C.0.01g potassium peroxydisulfate is added.Reaction 12 hours.By product centrifugal purification.
Embodiment 2
Experiment purpose and method: the core-shell quanta dots in order to characterize synthesis, the CdSe/ that the present embodiment is synthesized with embodiment 1
CdS quantum dot and core-shell quanta dots/polystyrene fluorescent microsphere are characterization object, and characterization content includes different shell numbers
CdSe/CdS quantum dot fluorescence emission spectrum, fluorescence quantum yield, fluorescent emission peak width and transmission electron microscope picture, nucleocapsid quantum
Point/polystyrene fluorescent microsphere fluorescence emission spectrum and different polystyrene dosages synthesize fluorescent microsphere transmission electron microscope picture, specifically
Experimental implementation is that details are not described herein again for standard test operation.
Experimental result:
It as shown in Figure 2,3, 4, can by controlling thermal cycle coupled method epitaxially grown quantum dot shell number on quantum dot core
To obtain the core-shell quanta dots that fluorescence emission peak changes from 548nm-750nm rule, and can by fluorescence quantum yield characterization
To find out, obtained core-shell quanta dots increasing with epitaxial growth shell, fluorescence quantum yield moves closer to 100%, has pole
High quantum yield.And can be seen that the continuation with epitaxial growth from transmission electron microscope picture, the average grain diameter of core-shell quanta dots
There is apparent increase.
As described in Figure 5, after the core-shell quanta dots of polystyrene package, the fluorescent microsphere fluorescence intensity of synthesis is compared with equivalent
Core-shell quanta dots decrease, fluorescence intensity loss about 15%, but the fluorescence intensity of the magnitude still meets the inspection of existing instrument
The demand of survey.By polystyrene dosage in reaction process, the fluorescent microsphere of different sizes can be synthesized, such as Fig. 6 institute
Show, the small figure polystyrene dosage of A-D is respectively 0.5mL, 0.8mL, 1mL, 1.2mL in Fig. 6, other implementation steps and embodiment 1
Identical, details are not described herein again.
The foregoing is only a preferred embodiment of the present invention, but scope of protection of the present invention is not limited thereto,
In the technical scope disclosed by the present invention, any changes or substitutions that can be easily thought of by anyone skilled in the art,
It should be covered by the protection scope of the present invention.
Claims (3)
1. a kind of core-shell quanta dots/polystyrene fluorescent microsphere preparation method, which is characterized in that the core-shell quanta dots are adopted
It is prepared with thermal cycle coupled method, and quantum dot is surface modified again using mercaptan, the core-shell quanta dots surface is repaired
The mercaptan ligand of decorations is alkyl hydrosulfide, and the mass ratio of quantum dot and alkyl hydrosulfide used in core-shell quanta dots ligand exchange is 1:
Quantum dot is embedded in polystyrene microsphere by (0.5-2) using emulsion polymerization, obtains core-shell quanta dots/polystyrene fluorescence
Microballoon, it is specific the preparation method is as follows:
Step 1: surfactant 2-20 parts, 0.2-2 parts of sodium bicarbonate, 2-30 parts of dispersing agent are weighed, is added in vial, then
It is added deionized water ultrasound 5-10 minutes, uniform mixed aqueous solution A is formed, using 100 parts of styrene as reference standard；
Step 2: weighing core-shell quanta dots 10-150 parts, 100 parts of styrene and 4-30 parts of tert-butyl acrylates are added, in ice bath
Middle ultrasonic 5 minutes, form uniform oil phase liquid B；
Step 3: magnetic agitation 10 minutes after both water solution A and oil phase liquid B are mixed, then ultrasound 5-20 minutes in ice bath,
Form stable microemulsion；
Step 4: microemulsion being transferred in there-necked flask, leads to the oxygen in 30 minutes removal there-necked flasks of nitrogen, is warming up to 60-80
DEG C, it is added initiator 1-30 parts, under magnetic stirring, is reacted 6-12 hours, by product centrifugal purification, obtains polystyrene fluorescence
Microballoon；
Wherein, by thermal cycle coupled method, the epitaxially grown quantum dot shell on quantum dot core is 1-16 to the core-shell quanta dots
Layer, the fluorescence spectra emission wavelength of core-shell quanta dots are 548nm-750nm.
2. a kind of preparation method of core-shell quanta dots/polystyrene fluorescent microsphere as described in claim 1, it is characterised in that:
Surfactant described in step 1 is ammonium lauryl sulfate, lauryl sodium sulfate, dodecyl sodium sulfate or 12
One of alkyl ethoxy sulfobetaines, the dispersing agent are the polyvinylpyrrolidone of each molecular weight.
3. a kind of preparation method of core-shell quanta dots/polystyrene fluorescent microsphere as described in claim 1, it is characterised in that:
Initiator described in step 4 is one of potassium peroxydisulfate or ammonium persulfate.
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| CN107722158B (en) * | 2017-10-10 | 2019-12-17 | 成都爱兴生物科技有限公司 | Monodisperse carboxyl modified quantum dot composite microsphere, and preparation method and application thereof |
| CN107966854A (en) * | 2017-11-23 | 2018-04-27 | 南通创亿达新材料股份有限公司 | The preparation method of quantum dot light emitting feature board in back light module unit structure |
| CN110590982A (en) * | 2019-10-08 | 2019-12-20 | 武汉珈源同创科技有限公司 | Quantum dot fluorescent microsphere and preparation method thereof |
| CN111088033B (en) * | 2019-12-25 | 2021-05-07 | 苏州为度生物技术有限公司 | Preparation method of monodisperse high-performance quantum dot fluorescent microspheres |
| CN116478694A (en) * | 2023-04-23 | 2023-07-25 | 天津大学 | Preparation and array method of polystyrene encapsulated nanocrystalline composite luminescent material |
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