CN1306003C - Process for preparing water soluble CdTe/CdS nuclear/shell type quantum point by microwave radiation reaction - Google Patents

Process for preparing water soluble CdTe/CdS nuclear/shell type quantum point by microwave radiation reaction Download PDF

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CN1306003C
CN1306003C CNB2005100255054A CN200510025505A CN1306003C CN 1306003 C CN1306003 C CN 1306003C CN B2005100255054 A CNB2005100255054 A CN B2005100255054A CN 200510025505 A CN200510025505 A CN 200510025505A CN 1306003 C CN1306003 C CN 1306003C
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cadmium
cdte
solution
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cds
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CN1693207A (en
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黄维
汪联辉
范曲立
何耀
陆昊婷
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Fudan University
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Fudan University
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Abstract

The present invention belongs to the technical field of nanometer materials and bioanalysis detection, which particularly relates to a microwave preparation method of water soluble CdTe/CdS nucleus/shell type quantum dots with high fluorescence quantum efficiency. An oxide of cadmium salt or cadmium is mixed with a water soluble sulfhydryl compound in a water phase, and nanometer crystal solution of cadmium telluride, which is prepared in advance, is injected into the mixture; consequently, CdTe/CdS precursor solution is obtained. The CdTe/CdS precursor solution is then placed in a special glass tube for microwave radiation, and a microwave radiation reaction is carried out in a microwave reactor; consequently, quantum dots and fluorescence quantum dots, which are of the CdTe/CdS nucleus/shell type, are prepared. The method is carried out completely in the water phase and has the advantages of safe and convenient operation, favorable water solubility and favorable stability of obtained products, and high fluorescence quantum efficiency. The method can be widely used in fluorescent markers for biological detection and analysis.

Description

The microwave preparation of a kind of water-soluble CdTe/CdS core/shell type quantum dot
Technical field
The invention belongs to nano material and bioanalysis detection technique field, be specifically related to the microwave preparation of a kind of high fluorescence quantum efficiency water-soluble CdTe/CdS core/shell type quantum dot.Be to be raw material, utilize microwave technology to prepare CdTe/CdS core/shell type quantum dot with cadmium salt (or its oxide compound, oxyhydroxide), sodium hydrogen telluride (or hydrogen telluride potassium, tellurium powder) and sodium sulphite (or potassium sulphide).
Background technology
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.Quantum dot has distinctive quantum size effect and surface effects, have many advantages with respect to traditional luminescent dye molecule with the nanocrystalline thing of marking: nanocrystalline exciting light spectrum width, emmission spectrum is narrow, symmetrical, the fluorescent emission wavelength can be by changing quantum dot size and component and being regulated, thereby the quantum dot of different size can be launched the fluorescence of different colours by the optical excitation of single wavelength, conveniently is used for the multi-color marking of multiple goal molecule.On the contrary, the fluorescence of multiple dyestuff but needs multiple laser to be excited, and this has not only increased experimental expenses, and makes analysis become complicated more.Nanocrystalline in addition luminous intensity height, photochemical stability is good, therefore quantum dot not only has purposes widely in optoelectronic information fields such as photoelectric device, photodiode, solid statelasers, and can be used as the novel fluorescent marker of a class, go out more and more tempting application prospect in biomedical fields such as molecular biology, immunobiology, clinical medicine.
The semiconductor nano crystal grain that needs in the practical application must have good luminescent properties (luminous efficiency height, fluorescence spectrum half-peak width), semiconductor nano crystal grain is applied to biomarker, also requires it to have biocompatibility.Therefore, the good water-soluble quantum dot of preparation luminescent properties becomes hot research in recent years.At present the report about the preparation of water soluble cadmium telluride quantum point is existing a lot, mainly contains common aqueous solution heating means (Rogach A.L, et.J.Phys.Chem.B, 2002,106,7177-7185; Rogach A.L, et.Adv.Mater, 2001,13,1684-1687), the pyritous hydrothermal method (Bai Yang, et.Adv.Mater, 2003,15,1712-1715) and directly the method for microwave radiation (Ren JC, et.Chem Comm, 2005,528-530).But the single cadmium telluride 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 cause, and quantum dot light emitting efficient is low, the fluorescence spectrum peak width at half height is too wide.Can be in single quantum dot surface epitaxy one deck lattice constant match, the wideer inorganic materials 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.At present about the report of this respect only limit to the common auxiliary photodegradative method of aqueous solution heating (Gao MY, et.Chem Mater, 2004,16,3853-3859), but chronic (several days to tens days) that need.
Summary of the invention
The objective of the invention is at problem recited above, propose a kind of operational safety, the microwave preparation of high fluorescence quantum efficiency water-soluble CdTe/CdS core/shell type quantum dot easily.
The preparation method of water-soluble CdTe provided by the invention/CdS core/shell type quantum dot, concrete steps are as follows:
1, preparation is as the sodium hydrogen telluride NaHTe or the hydrogen telluride potassium KHTe solution in tellurium source: the sodium borohydride NaBH that with mol ratio is 1.5: 1 to 5: 1 4Or POTASSIUM BOROHYDRIDE KBH 4Te places water with the tellurium powder, 0~30 degree centigrade of following standing and reacting 7~30 hours, obtains NaHTe or hydrogen telluride potassium KHTe solution;
2, oxide compound, oxyhydroxide and the water-soluble sulfhydryl compound solution of preparation 0.0005~0.1mol/L cadmium salt or cadmium, pH value to 7~13 of regulator solution, logical nitrogen removes oxygen, be heated to 70~120 degrees centigrade, inject NaHTe or KHTe solution, reacted 1~40 hour, obtain the CdTe quantum dot;
3, the concentration that water-soluble sulfhydryl compound is added as the cadmium source is oxide compound, oxyhydroxide and the sulfosalt solution of 0.0005~0.1mol/L cadmium salt or cadmium, and the CdTe quantum dot is injected in pH value to 7~13 of regulator solution, obtains the CdTe/CdS precursor solution;
4, the CdTe/CdS precursor solution is carried out microwave treatment: precursor solution is placed the microwave radiation special glass tube, in microwave reactor, carry out the microwave radiation reaction, obtain the water-soluble CdTe/CdS core/shell type quantum dot of different emission wavelengths, wherein, microwave heating condition is: microwave power 15W~1000W, heat-up times 30 second~5 hour, 70~200 degrees centigrade of Heating temperatures.
In the step 2 of aforesaid method, raw material cadmium source, sulfhydryl compound, tellurium source are Cd in molar ratio 2+: sulfhydryl compound: HTe -=1: (1.5~5): (0.3~0.7).
In the step 3 of aforesaid method, raw material cadmium source, sulfhydryl compound, sulphur source, cadmium telluride are Cd in molar ratio 2+: sulfhydryl compound: S 2-: CdTe=1: (1.5~8): (0.3~0.9): (0.05~3).
Oxide compound, the oxyhydroxide of cadmium salt of the present invention or cadmium comprise: Cadmium chloride fine powder, cadmium iodide, cadmium bromide, cadmium nitrate, Cadmium oxide, cadmium perchlorate, cadmium chlorate, cadmium iodate, Cadmium Sulphate, cadmium hydroxide or cadmium carbonate etc.; Described water miscible sulfhydryl compound comprises Thiovanic acid, thiohydracrylic acid, sulfydryl butyric acid, thioglycolate salt, mercapto propionate, halfcystine, Gelucystine, mercaptoethanol or mercaprol etc.; Described sulfosalt comprises sodium sulphite or potassium sulphide etc.
The present invention carries out at aqueous phase fully, operational safety, and easy rapidly, raw material is easy to get.Employing the present invention prepares the water-soluble CdTe/CdS core/shell type quantum dot fluorescence quantum yield height of gained, good stability, and have good water-solubility, can be used as fluorescent marker and be widely used in biological detection and analysis.
Description of drawings
Fig. 1 is the ultraviolet-fluorescence spectrum of the CdTe/CdS core/shell type quantum dot for preparing with the present invention.
Fig. 2 is the TEM and the HRTEM of the CdTe/CdS 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). the sodium hydrogen telluride preparation:
With 90.5 milligrams of NaBH 4Solid and 91.2 milligrams of Te powder are put in the little flask, add 3 ml waters, can obtain NaHTe solution in reaction under 10 degrees centigrade after 10 hours, and are standby;
(2) CdTe quantum dot preparation
With 22.5 milligrams of CdCl 2Be dissolved in 100 ml waters, add 0.03 milliliter of Thiovanic acid, regulate pH=9.5 with the NaOH solution of 0.5 mol, logical nitrogen 30 minutes is warming up to 100 degrees centigrade, injects 0.2 milliliter of NaHTe solution, reacts 3 hours, obtains the CdTe quantum dot solution;
(3) CdTe/CdS precursor solution preparation
With 18.5 milligrams of CdCl 2With 5.6 milligrams of Na 2S is dissolved in 100 ml waters, adds 0.06 milliliter of Thiovanic acid, regulates pH=10.5 with the NaOH appearance of 0.5 mol, injects 10 milliliters of CdTe quantum dot solutions, obtains the CdTe/CdS precursor solution;
(4) microwave radiation prepares CdTe/CdS core/shell type quantum dot
Resulting CdTe/CdS precursor solution is carried out the microwave radiation preparation, can obtain CdTe/CdS core/shell type quantum dot.The microwave radiation condition is as follows:
Microwave power: 50W; Temperature: 100 ℃; First program time: 5mins;
Embodiment 2
(1). the sodium hydrogen telluride preparation
With 90.7 milligrams of NaBH 4Solid and 127.6 milligrams of Te powder are put in the little flask, add 2.5 ml waters, can obtain NaHTe solution in reaction under 0 degree centigrade after 8 hours, and are standby;
(2) CdTe quantum dot preparation
With 30.0 milligrams of CdCl 2Be dissolved in 100 ml waters, add 0.05 milliliter of Thiovanic acid, regulate pH=9.0 with the NaOH solution of 0.5 mol, logical nitrogen 30 minutes is warming up to 100 degrees centigrade, injects 0.25 milliliter of NaHTe solution, reacts 5 hours, obtains the CdTe quantum dot solution;
(3) CdTe/CdS precursor solution preparation
With 25.9 milligrams of CdCl 2With 3.9 milligrams of Na 2S is dissolved in 100 ml waters, adds 0.03 milliliter of Thiovanic acid, regulates pH=8 with the NaOH solution of 0.5 mol, injects 20 milliliters of CdTe quantum dot solutions, obtains the CdTe/CdS precursor solution;
(4) the program controlling microwave radiation prepares CdTe/CdS core/shell type quantum dot
Resulting CdTe/CdS precursor solution is carried out the microwave radiation preparation, can obtain CdTe/CdS core/shell type quantum dot.The microwave radiation condition is as follows:
Microwave power: 300W; Temperature: 140 ℃; First program time: 1mins;
Embodiment 3
(1). the preparation of hydrogen telluride potassium
With 50.8 milligrams of KBH 4Solid and 63.8 milligrams of Te powder are put in the little flask, add 2 ml waters, can obtain KHTe solution in reaction under 20 degrees centigrade after 15 hours, and are standby;
(2) CdTe quantum dot preparation
With 25.6 milligrams of CdCl 2Be dissolved in 100 ml waters, add 0.018 milliliter of Thiovanic acid, regulate pH=8.5 with the NaOH solution of 0.5 mol, logical nitrogen 30 minutes is warming up to 90 degrees centigrade, injects 0.3 milliliter of KHTe solution, reacts 10 hours, obtains the CdTe quantum dot solution;
(3) CdTe/CdS precursor solution preparation
With 15.5 milligrams of CdCl 2With 5.0 milligrams of Na 2S is dissolved in 100 ml waters, adds 0.02 milliliter of Thiovanic acid, regulates pH=9.5 with the NaOH solution of 0.5 mol, injects 15 milliliters of CdTe quantum dot solutions, obtains the CdTe/CdS precursor solution;
(4) the program controlling microwave radiation prepares CdTe/CdS core/shell type quantum dot
Resulting CdTe/CdS precursor solution is carried out the microwave radiation preparation, can obtain CdTe/CdS core/shell type quantum dot.The microwave radiation condition is as follows:
Microwave power: 100W; Temperature: 130 ℃; First program time: 3mins;
Embodiment 4
(1). the sodium hydrogen telluride preparation:
With 98 milligrams of NaBH 4Solid and 115.6 milligrams of Te powder are put in the little flask, add 3 ml waters, can obtain NaHTe solution in reaction under 15 degrees centigrade after 11 hours, and are standby;
(2) CdTe quantum dot preparation
With 25.0 milligrams of CdCl 2Be dissolved in 100 ml waters, add 0.02 milliliter of Thiovanic acid, regulate pH=10.5 with the NaOH solution of 0.5 mol, logical nitrogen 30 minutes is warming up to 110 degrees centigrade, injects 0.2 milliliter of NaHTe solution, reacts 3.5 hours, obtains the CdTe quantum dot solution;
(3) CdTe/CdS precursor solution preparation
With 16.5 milligrams of CdCl 2With 3.6 milligrams of Na 2S is dissolved in 100 ml waters, adds 0.01 milliliter of Thiovanic acid, regulates pH=10.5 with the NaOH appearance of 0.5 mol, injects 10 milliliters of CdTe quantum dot solutions, obtains the CdTe/CdS precursor solution;
(4) microwave radiation prepares CdTe/CdS core/shell type quantum dot
Resulting CdTe/CdS precursor solution is carried out the microwave radiation preparation, can obtain CdTe/CdS core/shell type quantum dot.The microwave radiation condition is as follows:
Microwave power: 50W; Temperature: 80 ℃; First program time: 30mins;
Embodiment 5
(1). the preparation of hydrogen telluride potassium:
With 83.5 milligrams of KBH 4Solid and 92.6 milligrams of Te powder are put in the little flask, add 3 ml waters, can obtain KHTe solution in reaction under 10 degrees centigrade after 15 hours, and are standby;
(2) CdTe quantum dot preparation
With 26.9 milligrams of CdCl 2Be dissolved in 100 ml waters, add 0.07 milliliter of Thiovanic acid, regulate pH=11.0 with the NaOH solution of 0.5 mol, logical nitrogen 30 minutes is warming up to 100 degrees centigrade, injects 0.2 milliliter of KHTe solution, reacts 5 hours, obtains the CdTe quantum dot solution;
(3) CdTe/CdS precursor solution preparation
With 30.5 milligrams of CdCl 2With 7.8 milligrams of Na 2S is dissolved in 100 ml waters, adds 0.05 milliliter of Thiovanic acid, regulates pH=7.5 with the NaOH appearance of 0.5 mol, injects 10 milliliters of CdTe quantum dot solutions, obtains the CdTe/CdS precursor solution;
(4) microwave radiation prepares CdTe/CdS core/shell type quantum dot
Resulting CdTe/CdS precursor solution is carried out the microwave radiation preparation, can obtain CdTe/CdS core/shell type quantum dot.The microwave radiation condition is as follows:
Microwave power: 15W; Temperature: 70 ℃; First program time: 45mins;
By the method for the invention, can prepare the water-soluble CdTe/CdS core/shell type quantum dot of other type-stable agent.

Claims (4)

1, the microwave preparation of a kind of high fluorescence quantum efficiency water-soluble CdTe/CdS core/shell type quantum dot, its feature concrete steps are as follows:
(a) preparation is as the sodium hydrogen telluride NaHTe or the hydrogen telluride potassium KHTe solution in tellurium source: the sodium borohydride NaBH that with mol ratio is 1.5: 1 to 5: 1 4Or POTASSIUM BOROHYDRIDE KBH 4Te places water with the tellurium powder, 0~30 degree centigrade of following standing and reacting 7~30 hours, obtains NaHTe or hydrogen telluride potassium KHTe solution;
(b) oxide compound, oxyhydroxide and the water-soluble sulfhydryl compound solution of preparation 0.0005~0.1mol/L cadmium salt or cadmium, pH value to 7~13 of regulator solution, logical nitrogen removes oxygen, be heated to 70~120 degrees centigrade, inject NaHTe or KHTe solution, reacted 1 hour~40 hours, and obtained the CdTe quantum dot solution;
(c) oxide compound, oxyhydroxide and water-soluble sulfhydryl compound and the sulfosalt solution of preparation 0.0005~0.1mol/L cadmium salt or cadmium, the CdTe quantum dot is injected in pH value to 7~13 of regulator solution, obtains the CdTe/CdS precursor solution;
(d) the CdTe/CdS precursor solution is carried out microwave preparation, microwave heating condition is: microwave power 15W~1000W, heat-up times 30 second~5 hour, 70~200 degrees centigrade of Heating temperatures promptly obtain the water-soluble CdTe/CdS core/shell type quantum dot of different emission wavelengths;
Wherein, described water miscible sulfhydryl compound is Thiovanic acid, thiohydracrylic acid, sulfydryl butyric acid, thioglycolate salt, mercapto propionate, halfcystine or Gelucystine.
2, preparation method according to claim 1, it is characterized in that in the step (b): raw material cadmium source, sulfhydryl compound, tellurium source are Cd in molar ratio 2+: sulfhydryl compound: HTe -=1: (1.5~5): (0.3~0.7).
3, preparation method according to claim 1, it is characterized in that in the step (c): raw material cadmium source, sulfhydryl compound, sulphur source, cadmium telluride are Cd in molar ratio 2+: sulfhydryl compound: S 2-: CdTe=1: (1.5~8): (0.3~0.9): (0.05~3).
4,, it is characterized in that the oxide compound of described cadmium salt or cadmium, oxyhydroxide comprise: Cadmium chloride fine powder, cadmium iodide, cadmium bromide, cadmium nitrate, Cadmium oxide, cadmium perchlorate, cadmium chlorate, cadmium iodate, Cadmium Sulphate, cadmium hydroxide or cadmium carbonate according to the preparation method described in the claim 1; Described sulfosalt comprises sodium sulphite or potassium sulphide.
CNB2005100255054A 2005-04-28 2005-04-28 Process for preparing water soluble CdTe/CdS nuclear/shell type quantum point by microwave radiation reaction Expired - Fee Related CN1306003C (en)

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CN103965907A (en) * 2013-01-29 2014-08-06 华东理工大学 Near-infrared fluorescence emitting CdTe/CdS core/shell quantum dot, and preparation method thereof

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