CN102167977A - Preparation method of II-VI family water-soluble selenide semiconductor quantum dots - Google Patents
Preparation method of II-VI family water-soluble selenide semiconductor quantum dots Download PDFInfo
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Abstract
The invention provides a preparation method of II-VI family water-soluble selenide semiconductor quantum dots, which comprises the following specific steps: adding a stabilizer into solution containing soluble cadmium salt, soluble zinc salt or soluble mercury salt, then regulating the pH value of the solution to be be alkaline, then introducing hydrogen selenide gas under inert atmosphere, and reacting till the solution is pale yellow and transparent, thereby preparing solution of a precursor, wherein the molar ratio of the soluble cadmium salt, the soluble zinc salt or the soluble mercury salt to the stabilizer is 1: 3-1: 2. High-temperature and high-pressure fast growth is performed on the solution of the precursor, thereby preparing the II-VI family water-soluble selenide semiconductor quantum dots. For the preparation method, the operation is simple, the cost is low, the toxicity is small, and the prepared II-VI family water-soluble selenide semiconductor quantum dots can be directly used for biological fluorescent marking, clinical diagnosis and other experiments.
Description
Technical field
The present invention relates to the semiconductor material preparation field, relate to the preparation method of a kind of II-VI family soluble selenide semiconductor quantum dots particularly.
Background technology
Along with the development of material preparation technology, people can make nanocrystal with the several semiconductor material, if when its yardstick less than or when reaching its exciton Bohr radius, just be referred to as the quantum dot of this semiconductor material.Because quantum dot has quantum size effect, small-size effect and surface effects change raw-material physicochemical characteristic, as aspects such as light, magnetic, electricity, power, are its change of optical property more widely and use.CdSe, ZnSe, Cd(Zn) S, Cd(Zn) Se, Cd(Zn) group quantum dot such as Te, have special fluorescence emitting characteristics, be different from the fluorescence radiation organic dye, its fluorescence intensity height, fade or bleaching speed slow, the fluorescence spectrum peak is narrow, and is highly sensitive.Because quantum dot can be with and split into the quasi-molecule energy level, along with reducing of size, its light activated emission peak position blue shift.So its fluorescence spectrum peak of different size quantum dot is also different, means promptly to have the different fluorescence spectrums that is excited that under same excitation wavelength its spectral wavelength can cover certain wavelength region, makes exciting light spectral line continuous distribution.Different semiconductor-quantum-points, as II-VI compounds of group such as CdS, CdSe, CdTe, its luminescence exitation spectrum is in visible-range, but and wavelength continuous distribution, it can be under same exciting light sources, the crystalline quantum dot of the same race that the simultaneous excitation size is different can obtain the emmission spectrum of different visible lights, carries out the fluoroscopic examination of polynary series.These superior performances of quantum dot can substitute organic dye, play a great role in researchs such as biological stain, immunoassay, in situ hybridization and polychrome imaging.When it receives on the mcroorganism by certain coupling agent, can become an organism fluorescent marker class novelty, that be better than the organic dye marker.As described in patent CN200610018426.5, CN200610024086.7, CN200810123522 etc.
At present, the preparation quantum dot main path, a kind of is the high temperature organic synthesis, as document " [J]. Nano Lett; Vol.1,2001, pp.207 ~ 211 " " [J]. Angew. Chem. Int. Ed.; Vol.41,2002, pp.2368 ~ 2371 " etc. described.Another kind is that water at low temperature is combined to, as document " [J] .Phys. Chem. B. Vol.106,2002, pp.7177 ~ 7185 " " [J] .Mater Sci (2009) 44:285 – 292 " etc. described.In general, the water method is because water is cooked reaction medium, thereby production cost is lower, and toxicity is less, surface charge and surface properties adjustable height, and easily introduce different functional groups, therefore become the important method of synthetic quantum dot.Current, the method that water synthesizes selenide quantum dot in II-VI compounds of group all is to synthesize the direct and cadmium source reaction of NaHSe or selenite, in the growth that refluxes about 100 ℃, under normal atmosphere, this degree of scatter and fluorescence quantum yield to synthetic quantum dot has certain influence, and long reaction time.
It is more that the inventive method has overcome quantum dot impurities prepared in the prior art, there is more impurity level to influence fluorescence quantum efficiency, and the long defective of preparation time, the preparation method of a kind of II-VI family soluble selenide semiconductor quantum dots is provided, has the purity height, preparation time is short, the beneficial effect that fluorescence property is good.
Summary of the invention
The invention provides the preparation method of a kind of II-VI family soluble selenide semiconductor quantum dots, it is characterized in that described method in turn includes the following steps:
A) preparation precursor solution:
Regulate pH value to alkalescence add stablizer in the solution of solubility cadmium salt, soluble zinc salt or solubility mercury salt after, then, under inert atmosphere, feed hydrogen selenide gas, reaction to described solution is light yellow transparent, promptly makes described precursor solution; Wherein, the mol ratio of described solubility cadmium salt, soluble zinc salt or solubility mercury salt and described stablizer is 1:3-1:2;
B) growth of quantum dot:
Described precursor solution is carried out High Temperature High Pressure grow fast, make described II-VI family soluble selenide semiconductor quantum dots.
Among the preparation method of II of the present invention-VI family soluble selenide semiconductor quantum dots, the strength of solution of described solubility cadmium salt, soluble zinc salt or solubility mercury salt is 0.1-1mol/L; Described pH value is 9-10; Under 40-100 ℃ of temperature, feed described hydrogen selenide gas.
Among the preparation method of II of the present invention-VI family soluble selenide semiconductor quantum dots, described solubility cadmium salt is Cd(Ac)
2, CdCl
2, CdSO
4, Cd(NO
3)
2Or cadmium perchlorate; Described soluble zinc salt is Zn(Ac)
2, Zn Cl
2, Zn SO
4, Zn(NO
3)
2Or naphthenic acid zinc salt; Described solubility mercury salt is Hg SO
4
Among the preparation method of II of the present invention-VI family soluble selenide semiconductor quantum dots, described stablizer is mercaptan acid, mercaptoalcohol, mercapto hydramine or sulfydryl ammonia.Wherein, described mercaptan acid is Thiovanic acid, thiohydracrylic acid, mercaptoisobutyric acid, dimercaptosuccinic acid(DMSA), tetramethylolmethane four-3-mercaptopropionic acid ester or sulfydryl propane sulfonic acid; Described mercaptoalcohol is mercaptoethanol, dimercaprol dimercaptopropanol, 3-sulfydryl-2-butanols or 11-sulfydryl-1-undecyl alcohol; Described mercapto hydramine is mercaptoethylamine or mercapto ethanamide; Described sulfydryl ammonia is halfcystine or thioserine.
Among the preparation method of II of the present invention-VI family soluble selenide semiconductor quantum dots, the particle diameter of described II-VI family soluble selenide semiconductor quantum dots is 1.6-9.5nm.
The object of the invention be to provide a kind of at aqueous phase with gas H
2Se is the method that selenium source passes through Hydrothermal Preparation II-VI family soluble selenide semiconductor quantum dots, to improve group quantum dot fluorescence quantum yield, dispersing uniformity and to shorten preparation time.
For achieving the above object, the present invention adopts following technical scheme:
The method of a kind of gas phase-Hydrothermal Preparation II-VI family soluble selenide semiconductor quantum dots is characterized in that this method is the selenium source and the quantum dot to be prepared of growing fast with the hydrogen selenide gas under High Temperature High Pressure, concrete steps are as follows:
A) solubility cadmium salt, soluble zinc salt or solubility mercury salt is water-soluble, be mixed with the solution that concentration is 0.1 ~ 1mol/L; Add stablizer again, wherein the mol ratio of soluble salt and stablizer is 1:(2～3); Regulate pH value 9～10, be called solution A; Described stablizer is mercaptan acid, mercaptoalcohol, mercapto hydramine or sulfydryl ammonia; Then, under inert atmosphere, hydrogen selenide gas is fed in the step a gained solution A, under 40 ~ 100 ℃, react and become light yellow transparently to solution A by water white transparency, this solution is precursor solution;
B) gained precursor solution is put into the autoclave High Temperature High Pressure and grow fast, obtain the different II of size-VI family soluble selenide semiconductor quantum dots according to the difference of growth time.
Above-mentioned solubility cadmium salt has Cd(Ac)
2, CdCl
2, CdSO
4, Cd(NO
3)
2Or cadmium perchlorate; Described soluble zinc salt has Zn(Ac)
2, Zn Cl
2, Zn SO
4, Zn(NO
3)
2Or naphthenic acid zinc salt; Described solubility mercury salt is: Hg SO
4
Above-mentioned mercaptan acid is Thiovanic acid, thiohydracrylic acid, mercaptoisobutyric acid, dimercaptosuccinic acid(DMSA), tetramethylolmethane four-3-mercaptopropionic acid ester or sulfydryl propane sulfonic acid; Described mercaptoalcohol is mercaptoethanol, dimercaprol dimercaptopropanol, 3-sulfydryl-2-butanols or 11-sulfydryl-1-undecyl alcohol; Described mercapto hydramine is mercaptoethylamine or mercapto ethanamide; Described sulfydryl ammonia is halfcystine or thioserine.
Above-mentioned II-VI family soluble selenide semiconductor quantum dots particle diameter is 1.6～9.5nm.。
Compared with prior art, the present invention relates to a kind of method with gas phase-Hydrothermal Preparation II-VI family soluble selenide semiconductor quantum dots.This method specifically comprises the preparation of precursor solution, the steps such as growth of quantum dot.The present invention is that selenium source is (as H with gas
2Se gas), by feeding gas, reduced the impurity component of precursor solution, hydrothermal method is adopted in the growth of quantum dot, and preparation time has been shortened in the quick growth of quantum dot greatly under High Temperature High Pressure, prepared II-VI family soluble selenide semiconductor quantum dots, size distribution is uniformly dispersed from 1.6～9.5nm, and degree of crystallinity is good, few defective, the fluorescent yield height.Simultaneously preparation method of the present invention is simple to operate, and cost is low, and toxicity is little, and the prepared II-VI family soluble selenide semiconductor quantum dots that goes out can be directly used in experiments such as bioluminescence sign, clinical diagnosis.
Description of drawings
The uv-visible absorption spectra (slit is 1 nm) and fluorescence emission spectrum (PL) characteristic of the CdSe quantum dot (being abbreviated as MPA-QDs) that the thiohydracrylic acid that Fig. 1 prepares at 160 ℃ of different times of growing down for employing the inventive method coats.
Fig. 2 is the TEM figure of the portion C dSe quantum dot of the inventive method preparation.
Fig. 3 is the XRD figure spectrum of the CdSe quantum dot of the inventive method preparation.
Embodiment
In order to understand the present invention better, further illustrate content of the present invention below in conjunction with embodiment, but content of the present invention not only is confined to the following examples.Under the spirit and scope that do not deviate from inventive concept, variation and advantage that those skilled in the art can expect all are included among the present invention, and are protection domain with the appending claims.
The preparation of hydrogen selenide gas in the inventive method is carried out according to D.-W. Deng et al./Journal of Colloid and Interface Science 299 (2006) 225 – 232.
Embodiment 1:
1. with 0.48 mmole Cd (Ac)
22H
2O is dissolved in the 96ml water, adds 1.2 mmole thiohydracrylic acids, regulates pH value to about 9.5 with 1mol/L NaOH under stirring action, and solution is moved in the suitable three-necked bottle.
2. 0.63 mmole selenium powder and 1.26 mmole sodium borohydride 40ml deionized waters are added with nitrogen except that in the container of oxygen for some time; 0 ℃ of lower magnetic force stirring reaction 3 hours; obtain the Sodium Tetraborate precipitation of colourless transparent solution and adularescent, nitrogen protection is arranged in reaction process all the time.
3. get 2ml sodium borohydride solution and be positioned in the ice bath, when temperature is reduced to 0 ℃, dropwise a certain amount of 0.51mol/L sulphuric acid soln is joined in the sodium hydrogen selenide solution, violent reaction takes place in sulfuric acid and sodium hydrogen selenide immediately, generation be hydrogen selenide gas.
With hydrogen selenide gas under protection of nitrogen gas, follow nitrogen directly to feed and fill in the container of cadmium acetate and thiohydracrylic acid mixing solutions, 100 ℃ of temperature of reaction, solution immediately by original colourless become light yellow.This solution is precursor solution, and precursor solution does not have fluorescence.
5. precursor solution is transferred in the autoclave and grown 15 minutes at 160 ℃, the particle diameter of the CdSe quantum dot of preparation is 2.8nm.
As shown in Figure 1, present embodiment is that it is red shift with the prolongation of growth time in the uv-visible absorption spectra (slit is 1 nm) and fluorescence emission spectrum (PL) characteristic of the CdSe quantum dot (being abbreviated as MPA-QDs) of the thiohydracrylic acid coating of 160 ℃ of different time preparations of growing down.Wavelength when causing maximum absorption band moves to 598nm from 526nm, by experimental formula D=(1.6122 * 10-9) λ 4-(2.6575 * 10
-6) λ
3+ (1.6242 * 10
-3) λ
2-(0.4277 λ)+(41.57), the D that (D is a CdSe QDs diameter in the formula, and λ is ultraviolet-absorption spectrum first absorption peak wavelength peak position) calculates these several quantum dots is from 2.8nm to 4.6nm, and it is also more even to distribute; The quantum dot of different sizes can be excited by same monochromatic source (400nm) simultaneously, produces different fluorescence excitations peak, from 550nm to 630nm, reflects it under certain energy light action, after transition, and the red shift rule of different-grain diameter CdSe quantum radiation.
Figure 2 shows that the TEM figure of the portion C dSe quantum dot of present embodiment preparation.As can be seen from the figure Zhi Bei quantum dot even particle distribution, particle diameter is about 2.5nm.
Figure 3 shows that the XRD figure spectrum of the CdSe quantum dot of present embodiment preparation.According to the results of comparison of standard diffraction card (JCPDS#19-0191), prepared CdSe QDs has the face-centred cubic structure of zink sulphide type.3 diffraction peaks respectively corresponding (111), (220) and (311) diffraction surfaces.
Embodiment 2:
1. with 0.48 mmole ZnCl
2Be dissolved in the 96ml water, add 1.2 mmole Thiovanic acids, under stirring action, regulate pH value to about 9.5, solution is moved in the suitable three-necked bottle with 1mol/L NaOH.
2. dispose the Na of 0.02M
2Se solution has nitrogen protection all the time in layoutprocedure.
3. get 3mlNa
2Se solution is positioned in the ice bath, when temperature is reduced to 0 ℃, dropwise a certain amount of 0.51mol/L sulphuric acid soln is joined in this solution, and violent reaction takes place immediately for sulfuric acid and sodium selenide, generation be hydrogen selenide gas.
With hydrogen selenide gas under protection of nitrogen gas, follow nitrogen directly to feed and fill in the container of zinc chloride and Thiovanic acid mixing solutions, 90 ℃ of temperature of reaction, solution immediately by original colourless become light yellow.This solution is precursor solution, and precursor solution does not have fluorescence.
5. precursor solution is transferred in the autoclave and grown 30 minutes at 160 ℃, the particle diameter of the ZnSe quantum dot of preparation is 1.8nm.
Embodiment 3:
1. with 0.48 mmole Hg SO
4Be dissolved in the 96ml water, add 1.5 mmole mercaptoethylamines, under stirring action, regulate pH value to about 9.5, solution is moved in the suitable three-necked bottle with 1mol/L NaOH.
2. dispose the Al of 0.02M
2Se
3Solution has nitrogen protection all the time in layoutprocedure.
3. get the Al of 5ml 0.02M
2Se
3Solution is positioned in the ice bath, when temperature is reduced to 0 ℃, dropwise a certain amount of 0.51mol/L sulphuric acid soln is joined in this solution, and violent reaction takes place immediately for sulfuric acid and aluminum selenide, generation be hydrogen selenide gas.
With hydrogen selenide gas under protection of nitrogen gas, follow nitrogen directly to feed and fill in the container of cadmium nitrate and mercaptoethylamine mixing solutions, 70 ℃ of solution of temperature of reaction immediately by original colourless become light yellow.This solution is precursor solution, and precursor solution does not have fluorescence.
5. preceding body solution is transferred in the autoclave and grown 60 minutes at 160 ℃, the particle diameter of the HgSe quantum dot of preparation is 6.8nm.
Embodiment 4:
In this examples preparation method, add 1.8 mmole mercaptoethanols, other conditions are with embodiment 1, and the particle diameter of the CdSe quantum dot for preparing is 3.0nm.
Embodiment 5:
In this examples preparation method, add 1.6 mmole thioserines, other preparation conditions are with embodiment 2, and the particle diameter of the ZnSe quantum dot for preparing is 1.6nm.
Claims (5)
1. the preparation method of II-VI family soluble selenide semiconductor quantum dots is characterized in that described method in turn includes the following steps:
A). preparation precursor solution:
Regulate pH value to alkalescence add stablizer in the solution of solubility cadmium salt, soluble zinc salt or solubility mercury salt after, then, under inert atmosphere, feed hydrogen selenide gas, reaction to described solution is light yellow transparent, promptly makes described precursor solution; Wherein, the mol ratio of described solubility cadmium salt, soluble zinc salt or solubility mercury salt and described stablizer is 1:3-1:2;
B). the growth of quantum dot:
Described precursor solution is carried out High Temperature High Pressure grow fast, make described II-VI family soluble selenide semiconductor quantum dots.
2. the preparation method of II-VI family soluble selenide semiconductor quantum dots according to claim 1 is characterized in that the strength of solution of solubility cadmium salt described in the described step a), soluble zinc salt or solubility mercury salt is 0.1-1mol/L; Described pH value is 9-10; Under 40-100 ℃ of temperature, feed described hydrogen selenide gas.
3. the preparation method of II-VI family soluble selenide semiconductor quantum dots according to claim 1 is characterized in that described solubility cadmium salt is Cd(Ac)
2, CdCl
2, CdSO
4, Cd(NO
3)
2Or cadmium perchlorate; Described soluble zinc salt is Zn(Ac)
2, Zn Cl
2, Zn SO
4, Zn(NO
3)
2Or naphthenic acid zinc salt; Described solubility mercury salt is Hg SO
4
4. the preparation method of II-VI family soluble selenide semiconductor quantum dots according to claim 1 is characterized in that described stablizer is mercaptan acid, mercaptoalcohol, mercapto hydramine or sulfydryl ammonia; Wherein, described mercaptan acid is Thiovanic acid, thiohydracrylic acid, mercaptoisobutyric acid, dimercaptosuccinic acid(DMSA), tetramethylolmethane four-3-mercaptopropionic acid ester or sulfydryl propane sulfonic acid; Described mercaptoalcohol is mercaptoethanol, dimercaprol dimercaptopropanol, 3-sulfydryl-2-butanols or 11-sulfydryl-1-undecyl alcohol; Described mercapto hydramine is mercaptoethylamine or mercapto ethanamide; Described sulfydryl ammonia is halfcystine or thioserine.
5. the preparation method of II-VI family soluble selenide semiconductor quantum dots according to claim 1 is characterized in that the particle diameter of the II that obtains in the described step b)-VI family soluble selenide semiconductor quantum dots is 1.6-9.5nm.
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| CN103506139A (en) * | 2013-03-14 | 2014-01-15 | 江苏大学 | Preparation method and application of hydrothermal synthesized CdSe quantum dot photocatalyst |
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Application publication date: 20110831 |