CN106147748B - A kind of CdSeTe@SiO2Core-shell nano material and preparation method thereof - Google Patents
A kind of CdSeTe@SiO2Core-shell nano material and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a kind of CdSeTe@SiO2Core-shell nano material, it is by synthesizing quantum dot kernel, then the method that covers silica shells from level to level in core surface synthesizes.The invention also discloses CdSeTe@SiO above-mentioned2The preparation method of core-shell nano material.Compared with prior art, core-shell nano material scatter of the present invention is high, and can control the thickness of its shell, and smooth in appearance improves the application performance and application prospect of different-grain diameter nano silicon dioxide.Meanwhile this technological operation is accurate, the core shell nanoparticles size tunable of synthesis, smooth in appearance, dispersibility is high, and raw material is easy to get, at low cost.The product being prepared is the CdSeTe@SiO of different-grain diameter2Core-shell nano material is suitble to industrialized production.
Description
Technical field
The invention belongs to field of nanometer material technology, and in particular to a kind of CdSeTe@SiO2 core-shell nanos materials and its preparation side
Method.
Background technology
SiO2It is a kind of nontoxic, tasteless, free of contamination nonmetallic materials.SiO2Nano-particle has many unique performances
Be widely applied foreground, such as special photoelectricity effect property, high Magnetoresistance Phenomena, nonlinear resistance phenomenon still have under high temperature high-strength, high
The tough, characteristics such as stability is good.Additionally due to SiO2Have many advantages, such as optical transparence, chemical inertness, bio-compatibility, existing
For serving as key player in new material, composite nano material.
Quantum dot, also known as inorganic nanocrystal have broad application prospects in biological field.Quantum dot has unique
Optical characteristics：Emission peak wavelength can be adjusted by the size of composition material and grain size, and excitation wavelength range is very wide, be had larger
Stoke shift and narrow symmetrical fluorescence spectra.In addition, quantum dot also has preferable optical stability, with organic dyestuff
Molecule is compared, and has the advantages such as longer light emissioning cycle.
Coated with silica technique is one of most representational method in inorganic material modification.Earth silicon material system
Standby smooth compared with simple, surface and transparent and good biocompatibility.The nucleocapsid of coated with silica CdSeTe quantum dot synthesizing news
The advantages of nano material, new material combines CdSeTe quantum dots, provides guarantee for the biologic applications of silica.
Nano-meter SiO_22And CdSeTe quantum dots are fine since its respective feature has in fields such as medicine, bioengineering
Application.But there are no the example that both materials are combined to application, CdSeTe@SiO before2It can be in conjunction with the excellent of the two
Point has broad application prospects in every field such as bioengineering.Therefore research CdSeTe@SiO2Core-shell nano material has
Important theoretical realistic meaning.
Invention content
The technical problem to be solved in the present invention is to provide a kind of CdSeTe@SiO2 core-shell nano materials of different-grain diameter, with
Solve the problems such as of the existing technology ineffective
The present invention also technical problems to be solved are to provide the preparation method of above-mentioned CdSeTe@SiO2 core-shell nano materials.
In order to solve the above technical problems, the technical solution adopted by the present invention is as follows：
A kind of CdSeTe@SiO2The preparation method of core-shell nano material, it includes the following steps：
(1) exposed CdSeTe quantum dots is soluble in water, zinc is added into the aqueous solution of exposed CdSeTe quantum dots
PH is adjusted after salt and glutathione, reaction is stirred after adding ammonium hydroxide and ethyl orthosilicate, grain size is obtained through microwave reaction
CdSeTe@SiO less than 5nm2Solution；
Wherein, the CdSeTe@SiO2Refer to the core that CdSeTe quantum dot core surfaces are covered with silica shells
Shell nanometer material.
(2) grain size being prepared in step (1) is less than to the CdSeTe@SiO of 5nm2Solution filtering after it is soluble in water,
Arginine is added, carries out magnetic agitation (100~10000rpm), hexamethylene is added after being sufficiently mixed, keeps magnetic agitation (500
~10000rpm) in the case of heat up, add ethyl orthosilicate, removed after the completion of reaction layer solution up to grain size be 10~
The CdSeTe@SiO of 20nm2Solution；
(3) it is 10~20nm's that the grain size being prepared in step (2) is added into ethyl alcohol-ammonium hydroxide mixed system
CdSeTe@SiO2Solution and be kept stirring (500~10000rpm), the mixed liquor for adding ethyl orthosilicate and ethyl alcohol carries out
It is protected from light, product is soluble in water after centrifugation and washing, obtains the CdSeTe@SiO that grain size is 40~150nm2Solution.
In above-mentioned preparation method, water used is ultra-pure water.
In step (1), exposed CdSeTe quantum dots are in logical N2In the case of by CdCl2, Te powder and Se powder synthesis.
In step (1), it is dissolved in a concentration of 0.001~0.1mg/ml of the exposed CdSeTe quantum dots of water.
In step (1), the zinc salt is acetic acid dihydrate zinc, and the glutathione is reductive glutathione；Its
In, in the aqueous solution of exposed CdSeTe quantum dots, a concentration of 0.5~10mol/L of zinc salt, glutathione it is a concentration of
0.5~10mol/L.
In step (1), adjusting pH agents useful for same is NaOH aqueous solutions, and pH is adjusted to 11~12.
In step (1), the volume ratio of ammonium hydroxide and the aqueous solution of exposed CdSeTe quantum dots is 0.01~10ml：1L, just
The volume ratio of silester and the aqueous solution of exposed CdSeTe quantum dots is 1~100ml：1L；Wherein, the ammonium hydroxide is matter
The aqueous solution of the ammonia of score 25% is measured, the hybrid reaction time is 2~8h.
In step (1), the power of the microwave reaction is 200~300w, and the reaction time is 10~500min.
In step (2), grain size is less than the CdSeTe@SiO of 5nm2Solution and water volume ratio be 1：1~8；Wherein, mistake
Filter the CdSeTe@SiO that grain size is less than 5nm2Solution used in filter membrane aperture be 0.1~8 μm.
In step (2), after arginine is added, arginic a concentration of 0.004~0.5mmol/L, hexamethylene in mixed system
The additive amount of alkane is that 1~100ml is added in every liter of mixed system, and the additive amount of ethyl orthosilicate is to be added in every liter of mixed system
10~100ml；Wherein, two mixed systems above-mentioned refer both to before hexamethylene is added, the total volume of reaction system.
In step (2), the heating refers to that mixed system is warming up to 70~90 DEG C, reaction condition be 500~
Under the rotating speed of 10000rpm, 70~90 DEG C of 15~30h of reaction.
In step (2), all stirring operations should ensure that organic layer liquid level stabilizing.
In step (3), grain size is the CdSeTe@SiO of 10~20nm2Solution and ethyl alcohol-ammonium hydroxide mixed system volume
Than being 1：5~50；Wherein, the ethyl alcohol-ammonium hydroxide mixed system by ethyl alcohol and ammonium hydroxide with 20~50：1 volume ratio mixing and
At ammonium hydroxide is the aqueous solution for the ammonia that mass fraction is 25%.
In step (3), the mixed liquor of the ethyl orthosilicate and ethyl alcohol is by ethyl orthosilicate and ethyl alcohol with 1：2~8
Volume ratio is obtained through ultrasonic mixing；Wherein, ultrasonic power is 100~800W, and ultrasonic time is 5~15min.
In step (3), the mixed liquor of ethyl orthosilicate and ethyl alcohol and the CdSeTe@SiO that grain size is 10~20nm are added2It is molten
The volume ratio of the ethyl alcohol of liquid-ammonium hydroxide mixed system is 1：6~10.
In step (3), the mixed liquor of ethyl orthosilicate and ethyl alcohol is added in five times with identical interval time, interval time
For 5~20min.
In step (3), reaction condition is to react 15~30h under the rotating speed of 500~10000rpm.
In step (3), centrifugal method is that 8~15min is centrifuged under 8000~13000rpm.
In step (3), washing methods is cleaning 3 times, is cleaned with ethyl alcohol, is finally cleaned twice with ultra-pure water for the first time.
The CdSeTe@SiO that any one in above-mentioned preparation method is prepared2Core-shell nano material is also the present invention's
Within protection domain, including grain size is less than the CdSeTe@SiO of 5nm2, grain size be 10~20nm CdSeTe@SiO2It is with grain size
The CdSeTe@SiO of 40~150nm2, they are all the nano particles of nucleocapsid.
Advantageous effect：
Compared with prior art, the present invention has following advantage：
The present invention covers the method synthesis of silica shells from level to level by synthesizing quantum dot kernel, then in core surface
CdSeTe@SiO2Nucleus shell nanometer material, this core-shell nano material scatter is high, and can control the thickness of its shell,
Smooth in appearance improves the application performance and application prospect of different-grain diameter nano silicon dioxide.This technological operation is accurate, synthesis
Core shell nanoparticles size tunable, smooth in appearance, dispersibility is high, and raw material is easy to get, at low cost.The product being prepared is different grains
The CdSeTe@SiO of diameter2Core-shell nano material is suitble to industrialized production.
Description of the drawings
Fig. 1 is CdSeTe@SiO in embodiment 42Transmission electron microscope picture；
Fig. 2 is CdSeTe@SiO in embodiment 52Transmission electron microscope picture；
Fig. 3 is CdSeTe@SiO in embodiment 62Transmission electron microscope picture；
Fig. 4 is CdSeTe@SiO in embodiment 1 and embodiment 22Fluorescence spectra.
Specific implementation mode
According to following embodiments, the present invention may be better understood.However, as it will be easily appreciated by one skilled in the art that real
It applies content described in example and is merely to illustrate the present invention, without sheet described in detail in claims should will not be limited
Invention.
Embodiment 1：CdSeTe@SiO2(<5nm) synthesize
Exposed CdSeTe quantum dots are taken, are dissolved in 50ml ultra-pure waters, a concentration of 0.05mg/ml, solution is glassy yellow；Add
Acetic acid dihydrate zinc, the 0.31g reduced forms GSH (glutathione) for entering 0.11g, are carried out at the same time magnetic agitation；It is adjusted with NaOH molten
25% concentrated ammonia liquor of 0.8ml is added in the pH to 11.5 of liquid, and the TEOS (ethyl orthosilicate) of 5ml is added after stirring evenly in normal
Magnetic agitation reacts 4h under the conditions of temperature is protected from light.By the microwave reaction 30min of 300w after stirring 4h, Chinese red is finally obtained
CdSeTe@SiO2(<5nm) solution is specifically shown in Table 1.
Embodiment 2：CdSeTe@SiO2(<5nm) synthesize
Exposed CdSeTe quantum dots are taken, are dissolved in 100ml ultra-pure waters, a concentration of 0.06mg/ml, solution is glassy yellow；
Acetic acid dihydrate zinc, the 0.62g reduced forms GSH (glutathione) of 0.22g is added, is carried out at the same time magnetic agitation；It is adjusted with NaOH
25% concentrated ammonia liquor of 1.6ml is added in the pH to 11.2 of solution, and the TEOS (ethyl orthosilicate) of 10ml is added after stirring evenly
Magnetic agitation reacts 4h under the conditions of room temperature is protected from light.By the microwave reaction 2h of 300w after stirring 4h, Chinese red is finally obtained
CdSeTe@SiO2(<5nm) solution is specifically shown in Table 1.
Embodiment 3：CdSeTe@SiO2(10~20nm)
The CdSeTe@SiO that Example 1 obtains2(<5nm) solution 3ml, with 6ml is added after 0.22 μm of membrane filtration
Ultra-pure water be placed in the glass jar of 40ml, the L-arginine (arginine) of 0.12g is added, be added 1cm rotor carry out magnetic
Power stirring makes solution be uniformly mixed, and Chinese red is presented in solution at this time；The hexamethylene of 1ml is added, is positioned in 80 DEG C of baking oven,
Magnetic stirring speed is 600rpm simultaneously, keeps organic layer liquid level stabilizing；When 80 DEG C of the temperature rise of mixed solution, thereto
It is slowly added to the TEOS (ethyl orthosilicate) of 1.2ml, is kept stirring, constant temperature and organic layer liquid level stabilizing, is reacted for 24 hours, obtained
To the CdSeTe@SiO of clear, colorless2(10~20nm) solution, is specifically shown in Table 1.
Embodiment 4：CdSeTe@SiO2(10~20nm)
The CdSeTe@SiO that Example 2 obtains2(<5nm) solution 25ml, with 50ml is added after 0.22 μm of membrane filtration
Ultra-pure water be placed in the glass jar of 250ml, the L-arginine (arginine) of 0.90g is added, be added 2cm rotor carry out
Magnetic agitation makes solution be uniformly mixed, and Chinese red is presented in solution at this time；The hexamethylene of 10ml is added, is positioned over 80 DEG C of baking oven
In, while magnetic stirring speed is 600rpm, keeps organic layer liquid level stabilizing；When 80 DEG C of the temperature rise of mixed solution, to
It is wherein slowly added to the TEOS (ethyl orthosilicate) of 12.2ml, is kept stirring, constant temperature and organic layer liquid level stabilizing, is reacted
30h obtains the CdSeTe@SiO of clear, colorless2(10~20nm) solution, is specifically shown in Table 1.
Embodiment 5：CdSeTe@SiO2(45~60nm)
It takes 18ml ethyl alcohol that the 25% concentrated ammonia liquor mixing of 0.5ml, magnetic agitation 15min is added, adds 2ml embodiments
3CdSeTe@SiO2(10~20nm) solution, magnetic agitation 15min；Separately with 0.5mlTEOS (ethyl orthosilicate)+2ml ethyl alcohol
Mixed solution, point 5 times (each 0.5ml) are added to ethyl alcohol-ammonium hydroxide-CdSeTe@SiO after ultrasonic (400w) mixes 10min2(10~
20nm) in solution mixed liquor, addition magnetic agitation under the conditions of being protected from light under 10min, room temperature reacts 20h every time.It is taken out after reaction
Rotor removes supernatant after rotating speed 12000rpm centrifugations 10min, addition ethyl alcohol is taken to make later by reaction solution in centrifuging
CdSeTe@SiO2(45~60nm) redissolution is centrifuged again in ethanol, and supernatant is removed after rotating speed 12000rpm centrifugations 10min
Liquid adds the step for ultra-pure water repeats twice, finally by CdSeTe@SiO later2(45~60nm) is dissolved in ultra-pure water
It is settled to 10ml, is specifically shown in Table 1.
Embodiment 6：CdSeTe@SiO2(80~100nm)
It takes 18ml ethyl alcohol that the 25% concentrated ammonia liquor mixing of 0.5ml, magnetic agitation 15min is added, adds 0.5ml embodiments
4CdSeTe@SiO2(10~20nm) solution, magnetic agitation 10min；Separately with 0.5mlTEOS (ethyl orthosilicate)+2ml ethyl alcohol
Mixed solution, point 5 times (each 0.5ml) are added to ethyl alcohol-ammonium hydroxide-CdSeTe@SiO after ultrasonic (400w) mixes 15min2(10~
20nm) in solution mixed liquor, addition magnetic agitation under the conditions of being protected from light under 10min, room temperature reacts 20h every time.It is taken out after reaction
Rotor removes supernatant after rotating speed 10000rpm centrifugations 10min, addition ethyl alcohol is taken to make later by reaction solution in centrifuging
CdSeTe@SiO2(80~90nm) redissolution is centrifuged again in ethanol, and supernatant is removed after rotating speed 10000rpm centrifugations 10min
Liquid adds the step for ultra-pure water repeats twice, finally by CdSeTe@SiO later2(80~90nm) is dissolved in ultra-pure water
It is settled to 10ml, is specifically shown in Table 1.
Table 1
Embodiment 7：CdSeTe@SiO2Stability test
By the CdSeTe@SiO of different-grain diameter of the present invention2It is added in the solution of different electrolyte, measures CdSeTe@SiO2
Change of size, as shown in table 2.
Table 2
Claims (12)
1. a kind of CdSeTe@SiO2The preparation method of core-shell nano material, which is characterized in that it includes the following steps：
(1) exposed CdSeTe quantum dots is soluble in water, into the aqueous solution of exposed CdSeTe quantum dots be added zinc salt and
PH is adjusted after glutathione, adds hybrid reaction after ammonium hydroxide and ethyl orthosilicate, and grain size is obtained less than 5nm's through microwave reaction
CdSeTe@SiO2Solution；
(2) grain size being prepared in step (1) is less than to the CdSeTe@SiO of 5nm2Solution filtering after it is soluble in water, be added
Hexamethylene is added in arginine after being sufficiently mixed, heating, adds ethyl orthosilicate, layer solution is removed up to grain after the completion of reaction
Diameter is the CdSeTe@SiO of 10~20nm2Solution；
(3) the CdSeTe@SiO that the grain size being prepared in step (2) is 10~20nm are added into ethyl alcohol-ammonium hydroxide mixed system2
Solution, add ethyl orthosilicate and reacted with the mixed liquor of ethyl alcohol, product is soluble in water after centrifugation and washing, obtains
Grain size is the CdSeTe@SiO of 40~150nm2Solution；
In step (2), after arginine is added, arginic a concentration of 0.004~0.5mmol/L in mixed system, hexamethylene
Additive amount is that 1~100ml is added in every liter of mixed system, the additive amount of ethyl orthosilicate be addition 10 in every liter of mixed system~
100ml；
In step (3), grain size is the CdSeTe@SiO of 10~20nm2The volume ratio of solution and ethyl alcohol-ammonium hydroxide mixed system be 1：
5~50；Wherein, the ethyl alcohol-ammonium hydroxide mixed system by ethyl alcohol and ammonium hydroxide with 20~50：1 volume ratio mixes, ammonium hydroxide
For the aqueous solution for the ammonia that mass fraction is 25%.
2. preparation method according to claim 1, which is characterized in that in step (1), be dissolved in the exposed CdSeTe amounts of water
A concentration of 0.001~0.1mg/ml of son point.
3. preparation method according to claim 1, which is characterized in that in step (1), the zinc salt is acetic acid dihydrate
Zinc, the glutathione are reductive glutathione；Wherein, in the aqueous solution of exposed CdSeTe quantum dots, zinc salt it is dense
Degree is 0.5~10mol/L, a concentration of 0.5~10mol/L of glutathione.
4. preparation method according to claim 1, which is characterized in that in step (1), adjusting pH agents useful for same is NaOH water
Solution, pH are adjusted to 11~12.
5. preparation method according to claim 1, which is characterized in that in step (1), ammonium hydroxide and exposed CdSeTe quantum
The volume ratio of point aqueous solution is 0.01~10ml：1L, the volume ratio of ethyl orthosilicate and exposed CdSeTe quantum dot aqueous solutions
For 1~100ml：1L；Wherein, the ammonium hydroxide is the aqueous solution of the ammonia of mass fraction 25%, and the hybrid reaction time is 2~8h.
6. preparation method according to claim 1, which is characterized in that in step (1), the power of the microwave reaction is
200~300w, reaction time are 10~500min.
7. preparation method according to claim 1, which is characterized in that in step (2), grain size is less than the CdSeTe@of 5nm
SiO2Solution and water volume ratio be 1：1~8；Wherein, filtering grain size is less than the CdSeTe@SiO of 5nm2Solution used in filter membrane
Aperture be 0.1~8 μm.
8. preparation method according to claim 1, which is characterized in that in step (2), the heating refers to by mixture
System is warming up to 70~90 DEG C, and reaction condition is 70~90 DEG C of 15~30h of reaction under the rotating speed of 500~10000rpm.
9. preparation method according to claim 1, which is characterized in that in step (3), the ethyl orthosilicate and ethyl alcohol
Mixed liquor by ethyl orthosilicate and ethyl alcohol with 1：2~8 volume ratio is obtained through ultrasonic mixing；Wherein, ultrasonic power be 100~
800W, ultrasonic time are 5~15min.
10. preparation method according to claim 1, which is characterized in that in step (3), ethyl orthosilicate and ethyl alcohol it is mixed
It closes liquid and the CdSeTe@SiO that grain size is 10~20nm is added2The volume ratio of the ethyl alcohol of solution-ammonium hydroxide mixed system is 1：6~
10。
11. preparation method according to claim 1, which is characterized in that in step (3), reaction condition be 500~
Under the rotating speed of 10000rpm, 15~30h is reacted.
12. the CdSeTe@SiO that any one of claim 1~11 is prepared2Core-shell nano material.
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