CN1834198A - Prepn. process of ZnSe/ZnS kernel/shell type quantum points - Google Patents
Prepn. process of ZnSe/ZnS kernel/shell type quantum points Download PDFInfo
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- CN1834198A CN1834198A CN 200610024520 CN200610024520A CN1834198A CN 1834198 A CN1834198 A CN 1834198A CN 200610024520 CN200610024520 CN 200610024520 CN 200610024520 A CN200610024520 A CN 200610024520A CN 1834198 A CN1834198 A CN 1834198A
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Abstract
This invention discloses manufacture of water-soluble ZnSe/ZnS core/shell quantum dots by photodegradation together with program-controlled microwave radiation method. The method comprises the steps of: mixing zinc salt or zinc oxide with water-soluble thioglycollic acid in water phase, adding sodium selenium sulfite or potassium selenium sulfite formed by reaction of sodium sulfite or potassium sulfite with selenium powders, reacting to obtain ZnSe precursor solution, placing the solution in a glass tube for microwave radiation, controlling the microwave radiation by program to obtain ZnSe quantum dots, performing photodegradation to obtain water-soluble ZnSe/Zns core/shell quantum dots with a high fluorescence quantum efficiency. The method is completely operated in water phase, thus has such advantages as easy operation and low toxicity. The quantum dots manufactured have such advantages as high fluorescence quantum efficiency, high stability and good water solubility, and can be used as fluorescent labels and indicators for biological inspection and analysis.
Description
Technical field
The invention belongs to nano material and bioanalysis detection technique field, be specifically related to the photodegradation utility program controlled microwave preparation method of a kind of water soluble ZnSe/ZnS core/shell type quantum dot.Be to be raw material, utilize photodegradation utility program controlled microwave technology to prepare water soluble ZnSe/ZnS core/shell type quantum dot with zinc salt (or its oxide compound, oxyhydroxide) and sulfurous acid selenium sodium (or sulfurous acid selenium potassium, selenium powder).
Technical background
Quantum dot is a class by the elementary composition radius of II-VI family or III-V family less than or near the semiconductor nano crystal grain of exciton Bohr radius.Semiconductor nano has quantum size effect, and its optical property changes with size of particles and changes, and its luminous efficiency is compared also with body phase material and improved a lot simultaneously.Alivisatos in 1998 and Nie SM etc. respectively reported first utilize semiconductor nano to substitute organic fluorescent dye as the biomolecular labeling thing, successfully mark (Alivisatos.et, Science, 1998 such as iron transfer protein and immunoglobulin (Ig), 281,2013-2016; Nie SM.et, Science, 1998,281,2016-2018), indicated nanocrystalline huge applications potentiality in biological markers detection.The traditional biological fluorescence dye is commonly used the second of smelling ingot, rhodamine etc., can only carry out monochromatic mark, and its poor stability, and sensitivity is also restricted; And the fluorescence semiconductor nano material is compared with the bioluminescence dyestuff as fluorescent marker, has that fluorescent line is narrow, luminous efficiency is high, glow color is adjustable, can carry out series of advantages such as multi-color marking, and good light stability.
The semiconductor nano that needs in the practical application must have good luminescent properties (luminous efficiency height, fluorescence spectrum half-peak width, good stability), semiconductor nano is applied to biomarker, also requires it to have excellent biological compatibility.Therefore, the good water-soluble quantum dot of preparation luminescent properties becomes hot research in recent years.By scientist's continuous effort, can directly prepare quantum dot (Rogach A.L, et.J.Phys.Chem.B, 2002,106, the 7177-7185 of excellent property at present at aqueous phase by traditional hydrothermal method, high temperature hydrothermal method and microwave irradiation; Rogach A.L, et.Adv.Mater, 2001,13,1684-1687Bai Yang, et.Adv.Mater, 2003,15,1712-1715; Ren J.C, et.ChemComm, 2005,528-530), but type mainly concentrates on water-soluble CdTe quantum dots, and the water-soluble quantum dot of other types then seldom has report.This has limited the further widespread use of quantum dot to a great extent.Because the nontoxic characteristic of Zn, so the ZnSe quantum dot is compared the CdTe quantum dot and is had better Environmental compatibility.Adopt traditional hydrothermal method directly to prepare water soluble ZnSe quantum dots (Shavel A but only there is people such as Shavel to report at present at aqueous phase in 2004, et.J.Phys.Chem.B, 2004,108,5905-5908), and 2005 the disclosed microwave radiations of people such as Ji Cun prepare ZnSe quantum dot method (China national number of patent application: 2005100246938.8).But the single ZnSe quantum dot of preparation exists easy oxidation, instability, and there are shortcomings such as a large amount of non-radiative recombination centers in the surface, and these all greatly influence the quantum dot performance.Can be at single quantum dot surface epitaxy one deck lattice constant match, the wideer ZnS shell structure of band gap, thus the lip-deep a large amount of defectives of quantum dot eliminated to a certain extent, improve the luminescent properties of quantum dot.
Summary of the invention
The objective of the invention is at problem recited above, a kind of operational safety, easy water soluble ZnSe/ZnS core/shell type quantum dot light degraded utility program controlled microwave preparation method are provided.
Water soluble ZnSe provided by the invention/ZnS core/shell type quantum dot light degraded utility program controlled microwave preparation method, concrete steps are as follows:
1, preparation is as the sulfurous acid selenium sodium (Na of selenium source
2SeSO
3) or sulfurous acid selenium potassium (K
2SeSO
3) solution: the S-WAT (Na that with mol ratio is 15: 1 to 50: 1
2SO
3) or potassium sulfite (K
2SO
3) and selenium powder Se place water, 80～100 degrees centigrade of following standing and reacting 12～50 hours, obtain Na
2SeSO
3Or K
2SeSO
3Solution;
2, preparation is 0.0005～0.1mol/L zinc salt as the concentration in zinc source, or the oxide compound of zinc, or the oxyhydroxide of zinc and Thiovanic acid solution, and above-mentioned Na is injected in pH value to 5～9 of regulator solution
2SeSO
3Or K
2SeSO
3Solution obtains the ZnSe precursor solution, deposits under the nitrogen protection;
3, the ZnSe precursor solution is carried out the program controlling microwave heating, obtain the water soluble ZnSe quantum dots of different emission wavelengths, wherein microwave heating condition is: microwave power 15W～1000W, first programmed heating times 10 second～30 minute, 50～90 degrees centigrade of Heating temperatures, the second programmed heating time was 30 second～60 minute, 70～120 degrees centigrade of Heating temperatures;
Preferred heating condition is: microwave power 30W～500W, and first programmed heating times 30 second～10 minute, 70～90 degrees centigrade of Heating temperatures, the second programmed heating time was 2 minutes～10 minutes, 90～120 degrees centigrade of Heating temperatures;
4, place the ordinary light environment to carry out photodegradation the ZnSe quantum dot that obtains, obtain high fluorescence quantum efficiency water soluble ZnSe/ZnS core/shell type quantum dot.The photodegradation time generally can be 1 day-30 days.
Among the present invention, raw material zinc source, Thiovanic acid, selenium source are Zn in molar ratio
2+: Thiovanic acid: SeSO
3 2-=1: (1.5～5): (0.3～0.7).
Oxide compound, the oxyhydroxide of zinc salt described in the present invention or zinc comprise: zinc chloride, zinc iodide, zinc bromide, zinc nitrate, zinc oxide, zinc perchlorate, zinc chlorate, zinc iodate, zinc sulfate, zinc hydroxide or zinc carbonate.
The present invention carries out at aqueous phase fully, operational safety, easy, and toxicity is little, and materials safety is easy to get.The water soluble ZnSe of gained/ZnS core/shell type quantum dot fluorescence quantum yield height (～20%), good stability has good water-solubility, can be used as fluorescent marker and is widely used in biological detection and analysis.
Description of drawings
Fig. 1 is the UV spectrum of the ZnSe/ZnS core/shell type quantum dot for preparing with the present invention.
Fig. 2 is the fluorescence spectrum of the ZnSe/ZnS core/shell type quantum dot for preparing with the present invention.
Embodiment
In order to understand the content of patent of the present invention better, further specify the present invention below in conjunction with specific embodiment and legend.
Embodiment 1
(1) Na
2SeSO
3Preparation
Get 3.94g Na
2SO
3With 49.4mg Se powder, place single neck flask with 100ml, add the 50ml pure water, be heated to 90 ℃ under the nitrogen protection, reacted 35 hours, obtain Na
2SeSO
3Solution.
(2) ZnSe precursor solution preparation
With 17.2 milligrams of ZnCl
2Be dissolved in 100 ml waters, add 8.6 microlitre Thiovanic acids, regulate pH=6.5, inject 2 milliliters of Na with the NaOH solution of 0.5 mol
2SeSO
3Solution is as the ZnSe precursor solution;
(3) the program controlling microwave radiation prepares the ZnSe quantum dot
Resulting ZnSe precursor solution is carried out the program controlling microwave radiation, can obtain the ZnSe quantum dot.The time variable control condition is as follows:
First program microwave power: the 50W; First program temperature: 80 ℃; First program time: 30s;
Second program microwave power: the 80W; Second program temperature: 90 ℃; Second program time: 7min.
(4) photodegradation prepares ZnSe/ZnS core/shell type quantum dot
Place the ordinary light environment to carry out photodegradation 5 days the ZnSe quantum dot for preparing, obtain ZnSe/ZnS core/shell type quantum dot.
Embodiment 2
(1) Na
2SeSO
3Preparation
Get 1.5g Na
2SO
3With 21.5mg Se powder, place single neck flask with 25ml, add the 15ml pure water, be heated to 100 ℃ under the nitrogen protection, reacted 20 hours, obtain Na
2SeSO
3Solution.
(2) ZnSe precursor solution preparation
With 25.2 milligrams of ZnCl
2Be dissolved in 100 ml waters, add 11.2 microlitre Thiovanic acids, regulate pH=5.4, inject 3 milliliters of Na with the NaOH solution of 0.5 mol
2SeSO
3Solution is as the ZnSe precursor solution;
(3) the program controlling microwave radiation prepares the ZnSe quantum dot
Resulting ZnSe precursor solution is carried out the program controlling microwave radiation, can obtain the ZnSe quantum dot.The time variable control condition is as follows:
First program microwave power: the 70W; First program temperature: 75 ℃; First program time: 60s;
Second program microwave power: the 200W; Second program temperature: 110 ℃; Second program time: 3min.
(4) photodegradation prepares ZnSe/ZnS core/shell type quantum dot
Place the ordinary light environment to carry out photodegradation 10 days the ZnSe quantum dot for preparing, obtain ZnSe/ZnS core/shell type quantum dot.
Embodiment 3
(1) Na
2SeSO
3Preparation
Get 0.6g Na
2SO
3With 10.5mg Se powder, place single neck flask with 100ml, add the 50ml pure water, be heated to 80 ℃ under the nitrogen protection, reacted 35 hours, obtain Na
2SeSO
3Solution.
(2) ZnSe precursor solution preparation
With 36.5 milligrams of ZnCl
2Be dissolved in 100 ml waters, add 12.7 microlitre Thiovanic acids, regulate pH=7.5, inject 5 milliliters of Na with the NaOH solution of 0.5 mol
2SeSO
3Solution is as the ZnSe precursor solution;
(3) the program controlling microwave radiation prepares the ZnSe quantum dot
Resulting ZnSe precursor solution is carried out the program controlling microwave radiation, can obtain the ZnSe quantum dot.The time variable control condition is as follows:
First program microwave power: the 35W; First program temperature: 90 ℃; First program time: 30s;
Second program microwave power: the 300W; Second program temperature: 100 ℃; Second program time: 10min.
(4) photodegradation prepares ZnSe/ZnS core/shell type quantum dot
Place the ordinary light environment to carry out photodegradation 5 days the ZnSe quantum dot for preparing, obtain ZnSe/ZnS core/shell type quantum dot.
Embodiment 4
(1) K
2SeSO
3Preparation
Get 3.0g K
2SO
3With 28.6mg Se powder, place single neck flask with 50ml, add the 30ml pure water, be heated to 100 ℃ under the nitrogen protection, reacted 24 hours, obtain K
2SeSO
3Solution.
(2) ZnSe precursor solution preparation
With 15.6 milligrams of ZnCl
2Be dissolved in 100 ml waters, add 9.3 microlitre Thiovanic acids, regulate pH=7.3, inject 2.5 milliliters of K with the NaOH solution of 0.5 mol
2SeSO
3Solution is as the ZnSe precursor solution;
(3) the program controlling microwave radiation prepares the ZnSe quantum dot
Resulting ZnSe precursor solution is carried out the program controlling microwave radiation, can obtain the ZnSe quantum dot.The time variable control condition is as follows:
First program microwave power: the 30W; First program temperature: 70 ℃; First program time: 5min;
Second program microwave power: the 50W; Second program temperature: 120 ℃; Second program time: 5min.
(4) photodegradation prepares ZnSe/ZnS core/shell type quantum dot
Place the ordinary light environment to carry out photodegradation 8 days the ZnSe quantum dot for preparing, obtain ZnSe/ZnS core/shell type quantum dot.
Embodiment 5
(1) Na
2SeSO
3Preparation
Get 2.9g Na
2SO
3With 35.5mg Se powder, place single neck flask with 100ml, add the 50ml pure water, be heated to 90 ℃ under the nitrogen protection, reacted 25 hours, obtain Na
2SeSO
3Solution.
(2) ZnSe precursor solution preparation
With 53.2 milligrams of ZnCl
2Be dissolved in 100 ml waters, add 17.5 microlitre Thiovanic acids, regulate pH=6.5, inject 3.5 milliliters of Na with the NaOH solution of 0.5 mol
2SeSO
3Solution is as the ZnSe precursor solution;
(3) the program controlling microwave radiation prepares the ZnSe quantum dot
Resulting ZnSe precursor solution is carried out the program controlling microwave radiation, can obtain the ZnSe quantum dot.The time variable control condition is as follows:
First program microwave power: the 50W; First program temperature: 80 ℃; First program time: 3min;
Second program microwave power: the 100W; Second program temperature: 100 ℃; Second program time: 8min.
(4) photodegradation prepares ZnSe/ZnS core/shell type quantum dot
Place the ordinary light environment to carry out photodegradation 15 days the ZnSe quantum dot for preparing, obtain ZnSe/ZnS core/shell type quantum dot.
By the method for the invention, can prepare the water-soluble core/shell type quantum point of other type-stable.
The prepared ZnSe/ZnS core/shell type of the foregoing description quantum dot fluorescence quantum yield is more than 20%, and good stability, has good water-solubility, is applied as fluorescent marker in biological detection with in analyzing.
Claims (5)
1, the preparation method of a kind of water soluble ZnSe/ZnS core/shell type quantum dot is characterized in that adopting following step:
(a) preparation is as the Na of selenium source
2SeSO
3Or K
2SeSO
3Solution: the Na that with mol ratio is 15: 1 to 50: 1
2SO
3Or K
2SO
3Se places water with selenium powder, 80～100 degrees centigrade of following standing and reacting 12～50 hours, obtains Na
2SeSO
3Or K
2SeSO
3Solution;
(b) preparation is oxide compound, oxyhydroxide and the Thiovanic acid solution of 0.0005～0.1mol/L zinc salt or zinc as the concentration in zinc source, and above-mentioned Na is injected in pH value to 5～9 of regulator solution
2SeSO
3Or K
2SeSO
3Solution obtains the ZnSe precursor solution, deposits under the nitrogen protection;
(c) the ZnSe precursor solution is carried out the program controlling microwave heating, obtain the water soluble ZnSe quantum dots of different emission wavelengths, wherein microwave heating condition is: microwave power 15W～1000W, first programmed heating times 10 second～30 minute, 50～90 degrees centigrade of Heating temperatures, the second programmed heating time was 30 second～60 minute, 70～120 degrees centigrade of Heating temperatures;
(d) place the ordinary light environment to carry out photodegradation the ZnSe quantum dot that obtains, obtain high fluorescence quantum efficiency water soluble ZnSe/ZnS core/shell type quantum dot.
2, preparation method according to claim 1, its feature is in step (c), microwave heating condition is: microwave power 30W～500W, first programmed heating times 30 second～10 minute, 70～90 degrees centigrade of Heating temperatures, the second programmed heating time was 2 minutes～10 minutes, 90～120 degrees centigrade of Heating temperatures.
3, preparation method according to claim 1, it is characterized in that in the step (b): raw material zinc source, Thiovanic acid, selenium source are Zn in molar ratio
2+: Thiovanic acid: SeSO
3 2-=1: (1.5～5): (0.3～0.7).
4, preparation method according to claim 1 is characterized in that in the step (d): photodegradative time range is 1 day～30 days.
5,, it is characterized in that oxide compound, the oxyhydroxide of described zinc salt or zinc is zinc chloride, zinc iodide, zinc bromide, zinc nitrate, zinc oxide, zinc perchlorate, zinc chlorate, zinc iodate, zinc sulfate, zinc hydroxide or zinc carbonate according to the described preparation method of claim 1.
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Cited By (7)
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| WO2009099397A1 (en) * | 2008-02-04 | 2009-08-13 | Agency For Science, Technology And Research | Forming glutathione-capped and metal-doped zinc selenide/zinc sulfide core-shell quantum dots in aqueous solution |
| CN101476162B (en) * | 2008-12-24 | 2011-05-11 | 云南大学 | Method for synthesizing flower shaped ZnSe semiconductor nanocrystalline |
| CN101381600B (en) * | 2008-10-22 | 2012-02-01 | 中国科学院上海技术物理研究所 | Preparation method of biocompatible aqueous phase quantum point |
| US20120103789A1 (en) * | 2010-10-28 | 2012-05-03 | Syracuse University | Greener Synthesis of Nanoparticles Using Fine Tuned Hydrothermal Routes |
| CN104449661A (en) * | 2014-10-31 | 2015-03-25 | 苏州大学 | Novel information processing method based on DNA controlled quantum dots |
| CN108192620A (en) * | 2018-01-26 | 2018-06-22 | 鲁南煤化工研究院 | A kind of preparation method of high fluorescence quantum efficiency water-soluble CdTe S alloy quantum dots |
| WO2022134044A1 (en) * | 2020-12-25 | 2022-06-30 | 京东方科技集团股份有限公司 | Preparation method of znse quantum dot, znse quantum dot, znse structure, and display device |
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| CN1183999C (en) * | 2000-09-13 | 2005-01-12 | 王建毅 | Nm-class core-and-shell particles |
| EP1590171B1 (en) * | 2003-01-22 | 2011-06-08 | The Board Of Trustees Of The University Of Arkansas | Monodisperse core/shell and other complex structured nanocrystals and methods of preparing the same |
| CN1304524C (en) * | 2004-02-20 | 2007-03-14 | 财团法人工业技术研究院 | Process for preparating ZnX (X=S, Se, Te) quantum point |
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|---|---|---|---|---|
| WO2009099397A1 (en) * | 2008-02-04 | 2009-08-13 | Agency For Science, Technology And Research | Forming glutathione-capped and metal-doped zinc selenide/zinc sulfide core-shell quantum dots in aqueous solution |
| EP2262931A1 (en) * | 2008-02-04 | 2010-12-22 | Agency for Science, Technology And Research | Forming glutathione-capped and metal-doped zinc selenide/zinc sulfide core-shell quantum dots in aqueous solution |
| EP2262931A4 (en) * | 2008-02-04 | 2011-11-16 | Agency Science Tech & Res | Forming glutathione-capped and metal-doped zinc selenide/zinc sulfide core-shell quantum dots in aqueous solution |
| CN101381600B (en) * | 2008-10-22 | 2012-02-01 | 中国科学院上海技术物理研究所 | Preparation method of biocompatible aqueous phase quantum point |
| CN101476162B (en) * | 2008-12-24 | 2011-05-11 | 云南大学 | Method for synthesizing flower shaped ZnSe semiconductor nanocrystalline |
| US20120103789A1 (en) * | 2010-10-28 | 2012-05-03 | Syracuse University | Greener Synthesis of Nanoparticles Using Fine Tuned Hydrothermal Routes |
| CN104449661A (en) * | 2014-10-31 | 2015-03-25 | 苏州大学 | Novel information processing method based on DNA controlled quantum dots |
| CN108192620A (en) * | 2018-01-26 | 2018-06-22 | 鲁南煤化工研究院 | A kind of preparation method of high fluorescence quantum efficiency water-soluble CdTe S alloy quantum dots |
| WO2022134044A1 (en) * | 2020-12-25 | 2022-06-30 | 京东方科技集团股份有限公司 | Preparation method of znse quantum dot, znse quantum dot, znse structure, and display device |
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