CN106147748A - 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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- 238000002360 preparation method Methods 0.000 title claims abstract description 21
- 239000002086 nanomaterial Substances 0.000 title claims abstract description 18
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 50
- 229910052681 coesite Inorganic materials 0.000 claims abstract description 38
- 229910052906 cristobalite Inorganic materials 0.000 claims abstract description 38
- 229910052682 stishovite Inorganic materials 0.000 claims abstract description 38
- 229910052905 tridymite Inorganic materials 0.000 claims abstract description 38
- 239000002096 quantum dot Substances 0.000 claims abstract description 22
- 239000011258 core-shell material Substances 0.000 claims abstract description 16
- 239000000377 silicon dioxide Substances 0.000 claims abstract description 11
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 40
- 239000000243 solution Substances 0.000 claims description 39
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims description 29
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 claims description 26
- 238000006243 chemical reaction Methods 0.000 claims description 21
- 239000002245 particle Substances 0.000 claims description 21
- 229910021529 ammonia Inorganic materials 0.000 claims description 15
- RWSXRVCMGQZWBV-WDSKDSINSA-N glutathione Chemical compound OC(=O)[C@@H](N)CCC(=O)N[C@@H](CS)C(=O)NCC(O)=O RWSXRVCMGQZWBV-WDSKDSINSA-N 0.000 claims description 14
- 239000007864 aqueous solution Substances 0.000 claims description 12
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 11
- 229960003180 glutathione Drugs 0.000 claims description 10
- 239000007788 liquid Substances 0.000 claims description 10
- 235000003969 glutathione Nutrition 0.000 claims description 8
- 125000004836 hexamethylene group Chemical group [H]C([H])([*:2])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[*:1] 0.000 claims description 7
- ZXVOCOLRQJZVBW-UHFFFAOYSA-N azane;ethanol Chemical compound N.CCO ZXVOCOLRQJZVBW-UHFFFAOYSA-N 0.000 claims description 6
- 239000004475 Arginine Substances 0.000 claims description 5
- ODKSFYDXXFIFQN-UHFFFAOYSA-N arginine Natural products OC(=O)C(N)CCCNC(N)=N ODKSFYDXXFIFQN-UHFFFAOYSA-N 0.000 claims description 5
- 150000003751 zinc Chemical class 0.000 claims description 5
- 230000002829 reductive effect Effects 0.000 claims description 4
- HRSADIZPZPRZEI-UHFFFAOYSA-L zinc;diacetate;hydrate Chemical compound O.[Zn+2].CC([O-])=O.CC([O-])=O HRSADIZPZPRZEI-UHFFFAOYSA-L 0.000 claims description 4
- 239000000203 mixture Substances 0.000 claims description 3
- 238000005406 washing Methods 0.000 claims description 3
- 238000005119 centrifugation Methods 0.000 claims description 2
- 239000003795 chemical substances by application Substances 0.000 claims description 2
- 239000012528 membrane Substances 0.000 claims description 2
- 230000035484 reaction time Effects 0.000 claims description 2
- 238000010792 warming Methods 0.000 claims description 2
- JBJWASZNUJCEKT-UHFFFAOYSA-M sodium;hydroxide;hydrate Chemical group O.[OH-].[Na+] JBJWASZNUJCEKT-UHFFFAOYSA-M 0.000 claims 1
- 230000015572 biosynthetic process Effects 0.000 abstract description 9
- 238000003786 synthesis reaction Methods 0.000 abstract description 9
- 238000000034 method Methods 0.000 abstract description 7
- 239000002105 nanoparticle Substances 0.000 abstract description 4
- 238000004519 manufacturing process Methods 0.000 abstract description 2
- 239000005543 nano-size silicon particle Substances 0.000 abstract description 2
- 239000002994 raw material Substances 0.000 abstract description 2
- 238000013019 agitation Methods 0.000 description 14
- 238000003756 stirring Methods 0.000 description 11
- 229910021642 ultra pure water Inorganic materials 0.000 description 10
- 239000012498 ultrapure water Substances 0.000 description 10
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical group [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 9
- 239000000463 material Substances 0.000 description 7
- 239000012044 organic layer Substances 0.000 description 5
- 230000000087 stabilizing effect Effects 0.000 description 5
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 4
- 235000011114 ammonium hydroxide Nutrition 0.000 description 4
- LGZXYFMMLRYXLK-UHFFFAOYSA-N mercury(2+);sulfide Chemical compound [S-2].[Hg+2] LGZXYFMMLRYXLK-UHFFFAOYSA-N 0.000 description 4
- 239000011259 mixed solution Substances 0.000 description 4
- 238000002156 mixing Methods 0.000 description 4
- 239000006228 supernatant Substances 0.000 description 4
- 235000009697 arginine Nutrition 0.000 description 3
- 230000003287 optical effect Effects 0.000 description 3
- YKYOUMDCQGMQQO-UHFFFAOYSA-L cadmium dichloride Chemical compound Cl[Cd]Cl YKYOUMDCQGMQQO-UHFFFAOYSA-L 0.000 description 2
- 239000002131 composite material Substances 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000002189 fluorescence spectrum Methods 0.000 description 2
- 239000011521 glass Substances 0.000 description 2
- 238000005374 membrane filtration Methods 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 239000000376 reactant Substances 0.000 description 2
- OIXLLKLZKCBCPS-RZVRUWJTSA-N (2s)-2-azanyl-5-[bis(azanyl)methylideneamino]pentanoic acid Chemical compound OC(=O)[C@@H](N)CCCNC(N)=N.OC(=O)[C@@H](N)CCCNC(N)=N OIXLLKLZKCBCPS-RZVRUWJTSA-N 0.000 description 1
- ODKSFYDXXFIFQN-BYPYZUCNSA-N L-arginine Chemical compound OC(=O)[C@@H](N)CCCN=C(N)N ODKSFYDXXFIFQN-BYPYZUCNSA-N 0.000 description 1
- 229930064664 L-arginine Natural products 0.000 description 1
- 235000014852 L-arginine Nutrition 0.000 description 1
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 1
- PBJVVSIWWBZKBJ-UHFFFAOYSA-N [(4-aminophenyl)sulfonylamino]methanesulfonic acid;2-[bis(2-hydroxyethyl)amino]ethanol Chemical compound OCCN(CCO)CCO.NC1=CC=C(S(=O)(=O)NCS(O)(=O)=O)C=C1 PBJVVSIWWBZKBJ-UHFFFAOYSA-N 0.000 description 1
- 150000001335 aliphatic alkanes Chemical class 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 238000011109 contamination Methods 0.000 description 1
- 230000001186 cumulative effect Effects 0.000 description 1
- 239000000975 dye Substances 0.000 description 1
- 239000003792 electrolyte Substances 0.000 description 1
- 230000005284 excitation Effects 0.000 description 1
- 229910010272 inorganic material Inorganic materials 0.000 description 1
- 239000011147 inorganic material Substances 0.000 description 1
- 239000010410 layer Substances 0.000 description 1
- 239000002159 nanocrystal Substances 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 230000005622 photoelectricity Effects 0.000 description 1
- 238000010926 purge Methods 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 235000012239 silicon dioxide Nutrition 0.000 description 1
- 239000002210 silicon-based material Substances 0.000 description 1
- 238000013112 stability test Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
- 230000009967 tasteless effect Effects 0.000 description 1
- 239000011701 zinc Substances 0.000 description 1
- 229910052725 zinc Inorganic materials 0.000 description 1
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- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
- C09K11/02—Use of particular materials as binders, particle coatings or suspension media therefor
- C09K11/025—Use of particular materials as binders, particle coatings or suspension media therefor non-luminescent particle coatings or suspension media
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y20/00—Nanooptics, e.g. quantum optics or photonic crystals
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- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
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- C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
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- C09K11/88—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing selenium, tellurium or unspecified chalcogen elements
- C09K11/881—Chalcogenides
- C09K11/883—Chalcogenides with zinc or cadmium
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Abstract
The invention discloses a kind of CdSeTe@SiO2Core-shell nano material, it is by synthesis quantum dot kernel, then covers the method synthesis of silica shells from level to level at core surface and obtain.The invention also discloses aforesaid CdSeTe@SiO2The 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, smooth in appearance, improves application performance and the application prospect of different-grain diameter nano silicon.Meanwhile, this technological operation is accurate, the core shell nanoparticles size tunable of synthesis, smooth in appearance, and dispersibility is high, and raw material is easy to get, low cost.The product prepared is the CdSeTe@SiO of different-grain diameter2Core-shell nano material, is suitable for industrialized production.
Description
Technical field
The invention belongs to field of nanometer material technology, be specifically related to a kind of CdSeTe@SiO2 core-shell nano material and preparation side thereof
Method.
Background technology
SiO2It is a kind of nonmetallic materials nontoxic, tasteless, free of contamination.SiO2Nanoparticle has many unique performances
Be widely applied prospect, as special photoelectricity effect property, high Magnetoresistance Phenomena, nonlinear resistance phenomenon, still have high-strength, high under high temperature
The characteristics such as tough, good stability.Additionally due to SiO2Having the advantages such as optical transparence, chemical inertness, bio-compatibility, it is existing
Key player is served as in new material, composite nano material.
Quantum dot, also known as inorganic nanocrystal, has broad application prospects at biological field.Quantum dot has uniqueness
Optical characteristics: emission peak wavelength can be regulated by the size of composition material and particle diameter, and excitation wavelength scope is the widest, has bigger
Stoke shift and the fluorescence spectra of narrow symmetry.Additionally, 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 the most representational method during inorganic material is modified.Earth silicon material system
Standby relatively simple, smooth surface and transparent and good biocompatibility.The nucleocapsid of coated with silica CdSeTe quantum dot synthesizing new
Nano material, new material combines the advantage of CdSeTe quantum dot, and the biologic applications for silicon dioxide provides guarantee.
Nano-meter SiO_22And CdSeTe quantum dot has in the field such as medical science, biological engineering due to its respective feature very well
Application.But the most both materials are not combined the example of application, CdSeTe@SiO2Can excellent in conjunction with both
Point, all has broad application prospects in every field such as biological engineering.Therefore research CdSeTe@SiO2Core-shell nano material has
Important theoretical realistic meaning.
Summary of the invention
The technical problem to be solved in the present invention is to provide the CdSeTe@SiO2 core-shell nano material of a kind of different-grain diameter, with
The problems such as the poor effect that solution prior art exists
The present invention also to solve the technical problem that the preparation method being to provide above-mentioned CdSeTe@SiO2 core-shell nano material.
For solving above-mentioned technical problem, the technical solution used in the present invention is as follows:
A kind of CdSeTe@SiO2The preparation method of core-shell nano material, it comprises the steps:
(1) by soluble in water for exposed CdSeTe quantum dot, in the aqueous solution of exposed CdSeTe quantum dot, zinc is added
Regulate pH after salt and glutathion, stir hybrid reaction after adding ammonia and tetraethyl orthosilicate, obtain particle diameter through microwave reaction
CdSeTe@SiO less than 5nm2Solution；
Wherein, described CdSeTe@SiO2Refer to that CdSeTe quantum dot core surface is coated with the core of silica shells
Shell nanometer material.
(2) particle diameter prepared in step (1) is less than the CdSeTe@SiO of 5nm2Solution filter after soluble in water,
Add arginine, carry out magnetic agitation (100～10000rpm), add hexamethylene after being sufficiently mixed, keep magnetic agitation (500
～10000rpm) in the case of heat up, add tetraethyl orthosilicate, take off after having reacted layer solution i.e. obtain particle diameter be 10～
The CdSeTe@SiO of 20nm2Solution；
(3) adding the particle diameter prepared in step (2) in ethanol-ammonia mixed system is 10～20nm
CdSeTe@SiO2Solution and be kept stirring for (500～10000rpm), the mixed liquor adding tetraethyl orthosilicate and ethanol is carried out
Lucifuge react, product by centrifugation with washing after soluble in water, obtain the CdSeTe@SiO that particle diameter is 40～150nm2Solution.
In above-mentioned preparation method, water used is ultra-pure water.
In step (1), exposed CdSeTe quantum dot is at logical N2In the case of by CdCl2, Te powder and Se powder synthesis.
In step (1), the concentration of the exposed CdSeTe quantum dot being dissolved in water is 0.001～0.1mg/ml.
In step (1), described zinc salt is two acetate hydrate zinc, and described glutathion is reductive glutathione；Its
In, in the aqueous solution of exposed CdSeTe quantum dot, the concentration of zinc salt is 0.5～10mol/L, and the concentration of glutathion is
0.5～10mol/L.
In step (1), regulation pH agents useful for same is NaOH aqueous solution, pH regulator to 11～12.
In step (1), ammonia is 0.01～10ml:1L with the volume ratio of the aqueous solution of exposed CdSeTe quantum dot, just
Silester is 1～100ml:1L with the volume ratio of the aqueous solution of exposed CdSeTe quantum dot；Wherein, described ammonia is matter
The aqueous solution of the ammonia of amount mark 25%, the hybrid reaction time is 2～8h.
In step (1), the power of described microwave reaction is 200～300w, and the response time is 10～500min.
In step (2), particle diameter is less than the CdSeTe@SiO of 5nm2The volume ratio of solution and water be 1:1～8；Wherein, mistake
Filter particle diameter is less than the CdSeTe@SiO of 5nm2Solution used by the aperture of filter membrane be 0.1～8 μm.
In step (2), after adding arginine, in mixed system, arginic concentration is 0.004～0.5mmol/L, hexamethylene
The addition of alkane is to add 1～100ml in every liter of mixed system, and the addition of tetraethyl orthosilicate is to add in every liter of mixed system
10～100ml；Wherein, aforesaid two mixed systems refer both to before hexamethylene adds, the cumulative volume of reaction system.
In step (2), described intensification refers to be warming up to mixed system 70～90 DEG C, reaction condition be 500～
Under the rotating speed of 10000rpm, 70～90 DEG C of reactions 15～30h.
In step (2), all stirring operations should ensure that organic layer liquid level stabilizing.
In step (3), particle diameter is the CdSeTe@SiO of 10～20nm2The volume of solution and ethanol-ammonia mixed system
Ratio is 1:5～50；Wherein, described ethanol-ammonia mixed system by ethanol and ammonia so that the volume ratio of 20～50:1 mixes
Become, ammonia be mass fraction be the aqueous solution of the ammonia of 25%.
In step (3), the mixed liquor of described tetraethyl orthosilicate and ethanol by tetraethyl orthosilicate with ethanol with 1:2's～8
Volume ratio is mixed to get through ultrasonic；Wherein, ultrasonic power is 100～800W, and ultrasonic time is 5～15min.
In step (3), tetraethyl orthosilicate and the mixed liquor of ethanol and the CdSeTe@SiO that addition particle diameter is 10～20nm2Molten
The volume ratio of the ethanol of liquid-ammonia mixed system is 1:6～10.
In step (3), tetraethyl orthosilicate adds with identical interval time in five times with the mixed liquor of ethanol, interval time
It is 5～20min.
In step (3), reaction condition is under the rotating speed of 500～10000rpm, reacts 15～30h.
In step (3), centrifugal method is to be centrifuged 8～15min under 8000～13000rpm.
In step (3), washing methods is cleaning 3 times, first time ethanol purge, cleans with ultra-pure water for last twice.
The CdSeTe@SiO that any one in above-mentioned preparation method prepares2Core-shell nano material is also the present invention's
Within protection domain, it is less than the CdSeTe@SiO of 5nm including particle diameter2, particle diameter be 10～20nm CdSeTe@SiO2With particle diameter it is
The CdSeTe@SiO of 40～150nm2, they are all the nano-particle of nucleocapsid structure.
Beneficial effect:
Compared with prior art, the present invention has the advantage that
The present invention is by synthesis quantum dot kernel, then covers the method synthesis of silica shells from level to level at 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 application performance and the application prospect of different-grain diameter nano silicon.This technological operation is accurate, synthesis
Core shell nanoparticles size tunable, smooth in appearance, dispersibility is high, and raw material is easy to get, low cost.The product prepared is different grains
The CdSeTe@SiO in footpath2Core-shell nano material, is suitable for industrialized production.
Accompanying drawing explanation
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 spectrum figure.
Detailed description of the invention
According to following embodiment, the present invention be may be better understood.But, as it will be easily appreciated by one skilled in the art that reality
Execute the content described by example and be merely to illustrate the present invention, and should be also without limitation on basis described in detail in claims
Invention.
Embodiment 1:CdSeTe@SiO2(< 5nm) synthesis
Taking exposed CdSeTe quantum dot, be dissolved in 50ml ultra-pure water, concentration is 0.05mg/ml, and solution is glassy yellow；Add
Enter the two acetate hydrate zinc of 0.11g, 0.31g reduced form GSH (glutathion), carry out magnetic agitation simultaneously；Molten with NaOH regulation
The pH of liquid to 11.5, adds 25% strong aqua ammonia of 0.8ml, stirs and add the TEOS (tetraethyl orthosilicate) of 5ml afterwards in often
Magnetic agitation reaction 4h under the conditions of temperature lucifuge.By the microwave reaction 30min of 300w after stirring 4h, finally give Chinese red
CdSeTe@SiO2(< 5nm) solution, specifically it is shown in Table 1.
Embodiment 2:CdSeTe@SiO2(< 5nm) synthesis
Taking exposed CdSeTe quantum dot, be dissolved in 100ml ultra-pure water, concentration is 0.06mg/ml, and solution is glassy yellow；
Add the two acetate hydrate zinc of 0.22g, 0.62g reduced form GSH (glutathion), carry out magnetic agitation simultaneously；Regulate with NaOH
The pH of solution to 11.2, add 1.6ml 25% strong aqua ammonia, stir the TEOS (tetraethyl orthosilicate) adding 10ml afterwards in
Magnetic agitation reaction 4h under the conditions of room temperature lucifuge.By the microwave reaction 2h of 300w after stirring 4h, finally give Chinese red
CdSeTe@SiO2(< 5nm) solution, specifically it is shown in Table 1.
Embodiment 3:CdSeTe@SiO2(10～20nm)
The CdSeTe@SiO that Example 1 obtains2(< 5nm) solution 3ml, with adding 6ml's after the membrane filtration of 0.22 μm
Ultra-pure water is placed in the glass jar of 40ml, adds the L-arginine (arginine) of 0.12g, and the rotor adding 1cm carries out magnetic force
Stirring makes solution mix homogeneously, and now solution presents Chinese red；Add the hexamethylene of 1ml, be positioned in the baking oven of 80 DEG C, simultaneously
Magnetic agitation speed is 600rpm, keeps organic layer liquid level stabilizing；When the temperature of mixed solution rises 80 DEG C, the most slowly
Add the TEOS (tetraethyl orthosilicate) of 1.2ml, be kept stirring for, constant temperature and organic layer liquid level stabilizing, carry out reacting 24h, obtain
Bright colourless CdSeTe@SiO2(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 adding 50ml after the membrane filtration of 0.22 μm
Ultra-pure water be placed in the glass jar of 250ml, add 0.90g L-arginine (arginine), add 2cm rotor carry out magnetic
Power stirring makes solution mix homogeneously, and now solution presents Chinese red；Add the hexamethylene of 10ml, be positioned in the baking oven of 80 DEG C,
Magnetic agitation speed is 600rpm simultaneously, keeps organic layer liquid level stabilizing；When the temperature of mixed solution rises 80 DEG C, wherein
It is slowly added to the TEOS (tetraethyl orthosilicate) of 12.2ml, is kept stirring for, constant temperature and organic layer liquid level stabilizing, carry out reacting 30h,
CdSeTe@SiO to clear, colorless2(10～20nm) solution, is specifically shown in Table 1.
Embodiment 5:CdSeTe@SiO2(45～60nm)
Take 18ml ethanol add 0.5ml 25% strong aqua ammonia mixing, magnetic agitation 15min, add 2ml embodiment
3CdSeTe@SiO2(10～20nm) solution, magnetic agitation 15min；Separately join 0.5mlTEOS (tetraethyl orthosilicate)+2ml ethanol
Mixed solution, after ultrasonic (400w) mixing 10min, point 5 times (each 0.5ml) is added to ethanol-ammonia-CdSeTe@SiO2(10～
20nm) in solution mixed liquor, add under 10min, room temperature magnetic agitation reaction 20h under the conditions of lucifuge every time.Take out after reaction
Rotor, by reactant liquor in being centrifuged, rotating speed 12000rpm removes supernatant after being centrifuged 10min, takes addition ethanol afterwards and makes
CdSeTe@SiO2(45～60nm) are redissolved and are centrifuged, and rotating speed 12000rpm removes supernatant after being centrifuged 10min
Liquid, adds the step for that ultra-pure water repeats twice afterwards, finally by CdSeTe@SiO2(45～60nm) are dissolved in ultra-pure water
It is settled to 10ml, is specifically shown in Table 1.
Embodiment 6:CdSeTe@SiO2(80～100nm)
Take 18ml ethanol add 0.5ml 25% strong aqua ammonia mixing, magnetic agitation 15min, add 0.5ml embodiment
4CdSeTe@SiO2(10～20nm) solution, magnetic agitation 10min；Separately join 0.5mlTEOS (tetraethyl orthosilicate)+2ml ethanol
Mixed solution, after ultrasonic (400w) mixing 15min, point 5 times (each 0.5ml) is added to ethanol-ammonia-CdSeTe@SiO2(10～
20nm) in solution mixed liquor, add under 10min, room temperature magnetic agitation reaction 20h under the conditions of lucifuge every time.Take out after reaction
Rotor, by reactant liquor in being centrifuged, rotating speed 10000rpm removes supernatant after being centrifuged 10min, takes addition ethanol afterwards and makes
CdSeTe@SiO2(80～90nm) are redissolved and are centrifuged, and rotating speed 10000rpm removes supernatant after being centrifuged 10min
Liquid, adds the step for that ultra-pure water repeats twice afterwards, finally by CdSeTe@SiO2(80～90nm) are 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 invention2Add to the solution of different electrolyte, measure CdSeTe@SiO2
Change of size, as shown in table 2.
Table 2
Claims (14)
1. a CdSeTe SiO2The preparation method of core-shell nano material, it is characterised in that it comprises the steps:
(1) by soluble in water for exposed CdSeTe quantum dot, in the aqueous solution of exposed CdSeTe quantum dot add zinc salt and
Regulate pH after glutathion, add hybrid reaction after ammonia and tetraethyl orthosilicate, obtain particle diameter less than 5nm's through microwave reaction
CdSeTe@SiO2Solution；
(2) particle diameter prepared in step (1) is less than the CdSeTe@SiO of 5nm2Solution filter after soluble in water, add
Arginine, adds hexamethylene, heats up, add tetraethyl orthosilicate, take off layer solution and i.e. obtain grain after having reacted after being sufficiently mixed
Footpath is the CdSeTe@SiO of 10～20nm2Solution；
(3) in ethanol-ammonia mixed system, add the CdSeTe@SiO that particle diameter is 10～20nm prepared in step (2)2
Solution, the mixed liquor adding tetraethyl orthosilicate and ethanol reacts, product by centrifugation with washing after soluble in water, obtain
Particle diameter is the CdSeTe@SiO of 40～150nm2Solution.
Preparation method the most according to claim 1, it is characterised in that in step (1), is dissolved in the exposed CdSeTe amount of water
The concentration of son point is 0.001～0.1mg/ml.
Preparation method the most according to claim 1, it is characterised in that in step (1), described zinc salt is two acetate hydrate
Zinc, described glutathion is reductive glutathione；Wherein, in the aqueous solution of exposed CdSeTe quantum dot, zinc salt dense
Degree is 0.5～10mol/L, and the concentration of glutathion is 0.5～10mol/L.
Preparation method the most according to claim 1, it is characterised in that in step (1), regulation pH agents useful for same is NaOH water
Solution, pH regulator to 11～12.
Preparation method the most according to claim 1, it is characterised in that in step (1), ammonia and exposed CdSeTe quantum
The volume ratio of some aqueous solution is 0.01～10ml:1L, tetraethyl orthosilicate and the volume ratio of exposed CdSeTe quantum dot aqueous solution
It is 1～100ml:1L；Wherein, described ammonia is the aqueous solution of the ammonia of mass fraction 25%, and the hybrid reaction time is 2～8h.
Preparation method the most according to claim 1, it is characterised in that in step (1), the power of described microwave reaction is
200～300w, the response time is 10～500min.
Preparation method the most according to claim 1, it is characterised in that in step (2), particle diameter is less than the CdSeTe@of 5nm
SiO2The volume ratio of solution and water be 1:1～8；Wherein, the particle diameter CdSeTe@SiO less than 5nm is filtered2Solution used by filter membrane
Aperture be 0.1～8 μm.
Preparation method the most according to claim 1, it is characterised in that in step (2), after adding arginine, mixed system
In arginic concentration be 0.004～0.5mmol/L, the addition of hexamethylene be in every liter of mixed system add 1～100ml,
The addition of tetraethyl orthosilicate is to add 10～100ml in every liter of mixed system.
Preparation method the most according to claim 1, it is characterised in that in step (2), described intensification refers to mixture
System is warming up to 70～90 DEG C, and reaction condition is under the rotating speed of 500～10000rpm, 70～90 DEG C of reactions 15～30h.
Preparation method the most according to claim 1, it is characterised in that in step (3), particle diameter is 10～20nm
CdSeTe@SiO2The volume ratio of solution and ethanol-ammonia mixed system be 1:5～50；Wherein, described ethanol-ammonia mixes
Fit system is mixed with the volume ratio of 20～50:1 by ethanol and ammonia, ammonia be mass fraction be the water-soluble of the ammonia of 25%
Liquid.
11. preparation methoies according to claim 1, it is characterised in that in step (3), described tetraethyl orthosilicate and second
The mixed liquor of alcohol is mixed to get through ultrasonic with the volume ratio of 1:2～8 with ethanol by tetraethyl orthosilicate；Wherein, ultrasonic power is 100
～800W, ultrasonic time is 5～15min.
12. preparation methoies according to claim 1, it is characterised in that in step (3), tetraethyl orthosilicate is mixed with ethanol
Close liquid and add the CdSeTe@SiO that particle diameter is 10～20nm2The volume ratio of the ethanol of solution-ammonia mixed system be 1:6～
10。
13. preparation methoies according to claim 1, it is characterised in that in step (3), reaction condition be 500～
Under the rotating speed of 10000rpm, react 15～30h.
The CdSeTe@SiO that in 14. claim 1～13, any one prepares2Core-shell nano material.
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