CN103552999B - Method for preparing quantum dots at low temperature - Google Patents
Method for preparing quantum dots at low temperature Download PDFInfo
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- CN103552999B CN103552999B CN201310511736.0A CN201310511736A CN103552999B CN 103552999 B CN103552999 B CN 103552999B CN 201310511736 A CN201310511736 A CN 201310511736A CN 103552999 B CN103552999 B CN 103552999B
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Abstract
The invention discloses a method for preparing quantum dots at low temperature. The method disclosed by the invention comprises the following steps: at a room temperature of 40 DEG C, adding cadmium salts into an open system; then, dissolving the cadmium salts into secondary distilled water, and adding a stabilizer into the obtained object; adjusting the pH value of the obtained mixture by using sodium hydroxide; after a reducing agent is added, adjusting the obtained object to the previous pH value again; adding a selenium source or a tellurium source, and then adding an ammonia solution with a concentration of 25-28 wt % into the system; and finally, stirring the obtained product 1.0-30 hours at a room temperature of 40 DEG C so as to complete the reaction, wherein the concentration of the cadmium salts in the reaction system is 1.0*10<-4> mol/L-1.0*10<-2> mol/L; the concentration of ammonia in the reaction system is 0.25-2.0 mol/L; and the rate of substance amounts of the cadmium salts, the selenium source or tellurium source, the stabilizer and the reducing agent is 1:(0.02-0.5):(2.0-4.5):(2.0-80). According to the invention, the reducing agent and reaction conditions are mild, the operation is convenient, and the consumption of reagents is greatly reduced.
Description
Technical field
The invention belongs to the preparing technical field of semiconductor nano, be specifically related to the preparation method of cadmium selenide or cadmium telluride quantum dot under a kind of low temperature.
Background technology
Quantum dot, can be described as again nanocrystalline, is a kind of by II-VI group or the elementary composition nano particle of iii-v.Semiconductor-quantum-point shows the physical properties that the size different from corresponding body phase material and pattern rely on because of its special structure, caused in numerous Application Areass such as physics, chemistry, material, biomedicines and paid close attention to widely.And be widely used in the different sciemtifec and technical sphere such as biomarker, photodiode, laser apparatus and solar cell.
Compared with traditional fluorescent probe molecule, the IIB-VIA race semiconductor fluorescence quantum dots such as CdTe, CdSe have exciting light spectrum width, emmission spectrum is narrow, Color tunable, namely the nanocrystals quantum dots of different size can be sent the fluorescence of different colours by the optical excitation of single wavelength, and luminous intensity is high, and fluorescence lifetime is long, the advantages such as good light stability, obtain investigation and application widely at present in such as cell imaging etc.Synthetic method about quantum dot has more report, as sol-gel method, microwave irradiation, organometallic precursor method etc., wherein organometallic precursor method synthesizes the most frequently used method of high quality quantum dot, but this method due to phosphine class organic solvent with containing cadmium metal complex compound, toxicity is comparatively large, inflammable and explosive, makes synthesis condition harsh, and quantum dot can only be dispersed in nonpolar organic solvent, limit its investigation and application as biological labled material.
In aqueous phase, be mainly reductive agent with sodium borohydride or be that reductive agent synthesized semiconductor is nanocrystalline with hydrazine hydrate.The former reactive behavior is very high, and reaction should not control, and needs to consume a large amount of reductive agents, and there is the reaction product such as boric acid, and affect nanocrystalline quality, the latter is high toxic material, and it is very high to there is reactive behavior, the problem that reagent consumption is very large.Therefore, the nanocrystalline condition of suitability for industrialized production high-quality semiconductor is comparatively harsh, and cost is high.
Summary of the invention
The object of the invention is to for the problem such as the reductive agent hyperactivity existed in prior art, severe reaction conditions, reagent consumption be large, provide that a kind of reductive agent and reaction conditions are all very gentle, prepare under low temperature that simple operation, reagent consumption reduce greatly the method for quantum dot.
The inventive method comprises the steps: under room temperature to 40 DEG C condition, cadmium salt is added in unlimited system, then be dissolved in redistilled water, add stablizer wherein, with sodium hydroxide adjust ph, after adding reductive agent, be again adjusted to previous pH, add selenium source or tellurium source, in system, add the ammonia soln that concentration is 25wt% ~ 28wt% again, finally stir under room temperature to 40 DEG C condition and complete reaction in 1.0 ~ 30 hours; Wherein, the concentration of described cadmium salt in reaction system is 1.0 × 10
-4mol/L ~ 1.0 × 10
-2mol/L; The concentration of described ammoniacal liquor in reaction system is 0.25mol/L ~ 2.0mol/L; The amount of substance of described cadmium salt, selenium source or tellurium source, stablizer and reductive agent is than being 1:0.02 ~ 0.5:2.0 ~ 4.5:2.0 ~ 80.
Specifically, described cadmium salt is Cadmium chloride fine powder.
Specifically, described selenium source is selenite, SeO
2with the one in selenium powder.
Specifically, described tellurium source is tellurite and TeO
2in one.
Specifically, described stablizer is the one in halfcystine, Thiovanic acid, thiohydracrylic acid, dimercaptosuccinic acid, gsh and N-(2-mercaptopropionyl) glycine.
Specifically, described reductive agent is the compound of+4 valency sulphur; The compound of described+4 valency sulphur is NaHSO
3, Na
2sO
3with the one of Sodium Pyrosulfite.
Beneficial effect of the present invention is: (1) the present invention reductive agent used is very gentle, and reaction is easy to control, and reductive agent and ammoniacal liquor consumption low; (2) one-step synthesis is adopted, simple to operate, danger coefficient is low, experimental repeatability is better; (3) reaction conditions is gentle, and temperature of reaction is low, and raw material is easy to get, and is applicable to suitability for industrialized production.(4) the semiconductor nano fluorescence quantum efficiency of synthesizing is higher, and long-time storage fluorescence color stablizes (emission peak is at 430nm ~ 630nm).
Accompanying drawing explanation
Fig. 1 is CdTe quantum homogenization fluorescence spectrum prepared in the embodiment of the present invention 1 and uv-visible absorption spectroscopy figure.
Fig. 2 is CdTe quantum homogenization fluorescence spectrum prepared in the embodiment of the present invention 2 and uv-visible absorption spectroscopy figure.
Fig. 3 is CdTe quantum homogenization fluorescence spectrum prepared in the embodiment of the present invention 3 and uv-visible absorption spectroscopy figure.
Fig. 4 is CdTe quantum homogenization fluorescence spectrum prepared in the embodiment of the present invention 4 and uv-visible absorption spectroscopy figure.
Fig. 5 is CdTe quantum homogenization fluorescence spectrum prepared in the embodiment of the present invention 5 and uv-visible absorption spectroscopy figure.
Fig. 6 is CdTe quantum homogenization fluorescence spectrum prepared in the embodiment of the present invention 6 and uv-visible absorption spectroscopy figure.
Fig. 7 is CdTe quantum homogenization fluorescence spectrum prepared in the embodiment of the present invention 7 and uv-visible absorption spectroscopy figure.
Fig. 8 is CdTe quantum homogenization fluorescence spectrum prepared in the embodiment of the present invention 8 and uv-visible absorption spectroscopy figure.
Fig. 9 is CdTe quantum homogenization fluorescence spectrum prepared in the embodiment of the present invention 9 and uv-visible absorption spectroscopy figure.
Figure 10 is CdSe quantum dot homogenization fluorescence spectrum prepared in the embodiment of the present invention 10 and uv-visible absorption spectroscopy figure.
Figure 11 is CdSe quantum dot homogenization fluorescence spectrum prepared in the embodiment of the present invention 11 and uv-visible absorption spectroscopy figure.
Figure 12 is CdSe quantum dot homogenization fluorescence spectrum prepared in the embodiment of the present invention 12 and uv-visible absorption spectroscopy figure.
Figure 13 is CdSe quantum dot homogenization fluorescence spectrum prepared in the embodiment of the present invention 13 and uv-visible absorption spectroscopy figure.
Figure 14 is CdSe quantum dot homogenization fluorescence spectrum prepared in the embodiment of the present invention 14 and uv-visible absorption spectroscopy figure.
Figure 15 is CdSe quantum dot homogenization fluorescence spectrum prepared in the embodiment of the present invention 15 and uv-visible absorption spectroscopy figure.
Figure 16 is CdSe quantum dot homogenization fluorescence spectrum prepared in the embodiment of the present invention 16 and uv-visible absorption spectroscopy figure.
Figure 17 is CdSe quantum dot homogenization fluorescence spectrum prepared in the embodiment of the present invention 17 and uv-visible absorption spectroscopy figure.
Embodiment
Below in conjunction with drawings and Examples, the present invention is described in further detail, but the present invention is not limited to this.
It is 100mL that 100mL reaction system described in each example of the present invention refers to reaction system overall solution volume.Namely when overall solution volume is less than 100mL, then in system, add the NaOH solution consistent with system pH, make liquor capacity be 100mL.In example, water used is redistilled water.
Embodiment 1:
The CdCl of 1mmol is added in 100mL reaction system
22.5H
2o, 4mmol Thiovanic acid, magnetic force rapid stirring.Regulate pH=10 with sodium hydroxide solution, then add the Na of 1mmol
2sO
3, again regulate pH=10, then add the TeO of 0.5mmol
2, 2mL concentration be the ammoniacal liquor of 25wt%, at ambient temperature, magnetic agitation 4h.Water-soluble CdTe quantum dots homogenization uv-visible absorption spectroscopy figure prepared by the present embodiment and fluorescence spectrum figure is as shown in curve a, curve b in Fig. 1.
Embodiment 2:
The CdCl of 0.5mmol is added in 100mL reaction system
22.5H
2o, 1.2mmol thiohydracrylic acid, magnetic force rapid stirring.Regulate pH=11 with sodium hydroxide solution, then add the Na of 1mmol
2sO
3, again regulate pH=11, then add the TeO of 0.2mmol
2, 4mL concentration be the ammoniacal liquor of 25wt%, at ambient temperature, magnetic agitation 8h.Water-soluble CdTe quantum dots homogenization uv-visible absorption spectroscopy figure prepared by the present embodiment and fluorescence spectrum figure is as shown in curve a, curve b in Fig. 2.
Embodiment 3:
The CdCl of 1mmol is added in 100mL reaction system
22.5H
2o, 3.5mmol dimercaptosuccinic acid, magnetic force rapid stirring.PH=10 is regulated, the Na of 3mmol with sodium hydroxide solution
2sO
3, again regulate pH=10, then add the TeO of 0.3mmol
2, 3.5mL concentration be the ammoniacal liquor of 25wt%, under 40 DEG C of water bath condition, magnetic agitation 10h.Water-soluble CdTe quantum dots homogenization uv-visible absorption spectroscopy figure prepared by the present embodiment and fluorescence spectrum figure is as shown in curve a, curve b in Fig. 3.
Embodiment 4:
The CdCl of 0.1mmol is added in 100mL reaction system
22.5H
2o, 0.5mmol halfcystine, magnetic force rapid stirring.Regulate pH=12 with sodium hydroxide solution, then add the Na of 0.5mmol
2sO
3, again regulate pH=12, then add the TeO of 0.02mmol
2, 2mL concentration be the ammoniacal liquor of 25wt%, under 40 DEG C of water bath condition, magnetic agitation 12h.Water-soluble CdTe quantum dots homogenization uv-visible absorption spectroscopy figure prepared by the present embodiment and fluorescence spectrum figure is as shown in curve a, curve b in Fig. 4.
Embodiment 5:
The CdCl of 1mmol is added in 100mL reaction system
22.5H
2o, 2mmol Thiovanic acid, magnetic force rapid stirring.Regulate pH=9 with sodium hydroxide solution, then add the Na of 1mmol
2sO
3, again regulate pH=9, then add the TeO of 0.1mmol
2, 3mL concentration be the ammoniacal liquor of 25wt%, under 40 DEG C of water bath condition, magnetic agitation 14h.Water-soluble CdTe quantum dots homogenization uv-visible absorption spectroscopy figure prepared by the present embodiment and fluorescence spectrum figure is as shown in curve a, curve b in Fig. 5.
Embodiment 6:
The CdCl of 1mmol is added in 100mL reaction system
22.5H
2o, 4mmol Thiovanic acid, magnetic force rapid stirring.PH=11 is regulated, the Na of 1.5mmol with sodium hydroxide solution
2sO
3, again regulate pH=11, then add the TeO of 0.05mmol
2, 2mL concentration be the ammoniacal liquor of 25wt%, at ambient temperature, magnetic agitation 18h.Water-soluble CdTe quantum dots homogenization uv-visible absorption spectroscopy figure prepared by the present embodiment and fluorescence spectrum figure is as shown in curve a, curve b in Fig. 6.
Embodiment 7:
The CdCl of 0.5mmol is added in 100mL reaction system
22.5H
2o, 2.4mmol thiohydracrylic acid, magnetic force rapid stirring.Regulate pH=12 with sodium hydroxide solution, then add the Na of 0.5mmol
2sO
3, again regulate pH=12, then add the TeO of 0.01mmol
2, 6mL concentration be the ammoniacal liquor of 25wt%, under 40 DEG C of water bath condition, magnetic agitation 22h.Water-soluble CdTe quantum dots homogenization uv-visible absorption spectroscopy figure prepared by the present embodiment and fluorescence spectrum figure is as shown in curve a, curve b in Fig. 7.
Embodiment 8:
The CdCl of 0.2mmol is added in 100mL reaction system
22.5H
2o, 0.48mmol Thiovanic acid, magnetic force rapid stirring.Regulate pH=9 with sodium hydroxide solution, then add the Sodium Pyrosulfite of 1mmol, again regulate pH=9, then add the Na of 0.05mmol
2teO
3, 4mL concentration be the ammoniacal liquor of 25wt%, under 40 DEG C of water bath condition, magnetic agitation 22h.Water-soluble CdTe quantum dots homogenization uv-visible absorption spectroscopy figure prepared by the present embodiment and fluorescence spectrum figure is as shown in curve a, curve b in Fig. 8.
Embodiment 9:
The CdCl of 0.1mmol is added in 100mL reaction system
22.5H
2o, 0.39mmol halfcystine, magnetic force rapid stirring.Regulate pH=11 with sodium hydroxide solution, then add the NaHSO of 1mmol
3, again regulate pH=11, then add the Na of 0.05mmol
2teO
3, 3mL concentration be the ammoniacal liquor of 25wt%, at ambient temperature, magnetic agitation 24h.Water-soluble CdTe quantum dots homogenization uv-visible absorption spectroscopy figure prepared by the present embodiment and fluorescence spectrum figure is as shown in curve a, curve b in Fig. 9.
Embodiment 10:
The CdCl of 0.01mmol is added in 100mL reaction system
22.5H
2o, 0.04mmol Thiovanic acid, magnetic force rapid stirring.Regulate pH=13 with sodium hydroxide solution, then add the Na of 0.020mmol
2sO
3, again regulate pH=13, then add the SeO of 0.002mmol
2, 2mL concentration be the ammoniacal liquor of 25wt%, at room temperature, magnetic agitation 2h.Water-soluble CdSe quantum dot homogenization uv-visible absorption spectroscopy figure prepared by the present embodiment and fluorescence spectrum figure is as shown in curve a, curve b in Figure 10.
Embodiment 11:
Under room temperature condition, in 100mL reaction system, add the CdCl of 0.1mmol
22.5H
2o, 0.4mmol thiohydracrylic acid, under magnetic force rapid stirring.Regulate pH=11 with sodium hydroxide solution, then add the Na of 0.4mmol
2sO
3, again regulate pH=11, then add the SeO of 0.05mmol
2, 2mL concentration be the ammoniacal liquor of 25wt%, at room temperature, magnetic agitation 4h.Water-soluble CdSe quantum dot homogenization uv-visible absorption spectroscopy figure prepared by the present embodiment and fluorescence spectrum figure is as shown in curve a, curve b in Figure 11.
Embodiment 12:
The CdCl of 0.1mmol is added in 100mL reaction system
22.5H
2o, 0.5mmol gsh, magnetic force rapid stirring.Regulate pH=13 with sodium hydroxide solution, then add the Na of 0.5mmol
2sO
3, again regulate pH=13, then add the SeO of 0.005mmol
2, 7mL concentration be the ammoniacal liquor of 25wt%, under 40 DEG C of conditions, magnetic agitation 8h.Water-soluble CdSe quantum dot homogenization uv-visible absorption spectroscopy figure prepared by the present embodiment and fluorescence spectrum figure is as shown in curve a, curve b in Figure 12.
Embodiment 13:
The CdCl of 0.1mmol is added in 100mL reaction system
22.5H
2o, 0.35mmol halfcystine, magnetic force rapid stirring.Regulate pH=11 with sodium hydroxide solution, then add the Na of 1mmol
2sO
3, again regulate pH=11, then add the SeO of 0.05mmol
2, 5mL concentration be the ammoniacal liquor of 25wt%, at ambient temperature, magnetic agitation 14h.Water-soluble CdSe quantum dot homogenization uv-visible absorption spectroscopy figure prepared by the present embodiment and fluorescence spectrum figure is as shown in curve a, curve b in Figure 13.
Embodiment 14:
Under 40 DEG C of conditions, in 100mL reaction system, add the CdCl of 1mmol
22.5H
2o, 3.0mmol Thiovanic acid, magnetic force rapid stirring.Regulate pH=12 with sodium hydroxide solution, then add the NaHSO of 2.5mmol
3, again regulate pH=12, then add the Se powder of 0.3mmol, the concentration of 3mL is the ammoniacal liquor of 25wt%, magnetic agitation 6h.Water-soluble CdSe quantum dot homogenization uv-visible absorption spectroscopy figure prepared by the present embodiment and fluorescence spectrum figure is as shown in curve a, curve b in Figure 14.
Embodiment 15:
The CdCl of 0.5mmol is added in 100mL reaction system
22.5H
2o, 2mmolN-(2-mercaptopropionyl) glycine, magnetic force rapid stirring.Regulate pH=11 with sodium hydroxide solution, then add the Sodium Pyrosulfite of 0.5mmol, again regulate pH=11, then add the SeO of 0.02mmol
2, 4mL concentration be the ammoniacal liquor of 25wt%, at ambient temperature, magnetic agitation 21h.Water-soluble CdSe quantum dot homogenization uv-visible absorption spectroscopy figure prepared by the present embodiment and fluorescence spectrum figure is as shown in curve a, curve b in Figure 15.
Embodiment 16:
The CdCl of 0.04mmol is added in 100mL reaction system
22.5H
2o, 0.16mmol Thiovanic acid, magnetic force rapid stirring.Regulate pH=9 with sodium hydroxide solution, then add the Na of 1mmol
2sO
3, again regulate pH=9, then add the SeO of 0.01mmol
2, 2mL concentration be the ammoniacal liquor of 25wt%, under 40 DEG C of conditions, magnetic agitation 26h.Water-soluble CdSe quantum dot homogenization uv-visible absorption spectroscopy figure prepared by the present embodiment and fluorescence spectrum figure is as shown in curve a, curve b in Figure 16.
Embodiment 17:
The CdCl of 0.1mmol is added in 100mL reaction system
22.5H
2o, 1mmol Thiovanic acid, magnetic force rapid stirring.PH=11 is regulated, the Na of 1.5mmol with sodium hydroxide solution
2sO
3, again regulate pH=11, then add the SeO of 0.04mmol
2, 2mL concentration be the ammoniacal liquor of 25wt%, at ambient temperature, magnetic agitation 30h.Water-soluble CdSe quantum dot homogenization uv-visible absorption spectroscopy figure prepared by the present embodiment and fluorescence spectrum figure is as shown in curve a, curve b in Figure 17.
Claims (6)
1. under a low temperature, prepare the method for quantum dot, it is characterized in that comprising the steps: under room temperature to 40 DEG C condition, cadmium salt is added in unlimited system, then be dissolved in redistilled water, added stablizer wherein, with sodium hydroxide adjust ph, previous pH is again adjusted to after adding reductive agent, add selenium source or tellurium source, then in system, add the ammonia soln that concentration is 25wt% ~ 28wt%, finally stir under room temperature to 40 DEG C condition and complete reaction in 1.0 ~ 30 hours; Wherein, the concentration of described cadmium salt in reaction system is 1.0 × 10
-4mol/L ~ 1.0 × 10
-2mol/L; The concentration of described ammoniacal liquor in reaction system is 0.25mol/L ~ 2.0mol/L; The amount of substance of described cadmium salt, selenium source or tellurium source, stablizer and reductive agent is than being 1:0.02 ~ 0.5:2.0 ~ 5:1.0 ~ 25;
Described reductive agent is the compound of+4 valency sulphur.
2. prepare the method for quantum dot according to claim 1 under low temperature, it is characterized in that: described cadmium salt is Cadmium chloride fine powder.
3. prepare the method for quantum dot according to claim 1 under low temperature, it is characterized in that: described selenium source is selenite, SeO
2with the one in selenium powder.
4. prepare the method for quantum dot according to claim 1 under low temperature, it is characterized in that: described tellurium source is tellurite and TeO
2in one.
5. prepare the method for quantum dot according to claim 1 under low temperature, it is characterized in that: described stablizer is the one in halfcystine, Thiovanic acid, thiohydracrylic acid, dimercaptosuccinic acid, gsh and N-(2-mercaptopropionyl) glycine.
6. prepare the method for quantum dot according to claim 1 under low temperature, it is characterized in that: the compound of described+4 valency sulphur is NaHSO
3, Na
2sO
3with the one of Sodium Pyrosulfite.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101870459A (en) * | 2010-06-11 | 2010-10-27 | 山东大学 | Method for preparing water-soluble CdTe quantum dots |
| CN102060273A (en) * | 2010-11-05 | 2011-05-18 | 桂林理工大学 | Method for preparing I-III-VI group semiconductor material through solvothermal synthesis in constant pressure open system |
| CN102634342A (en) * | 2012-03-31 | 2012-08-15 | 华东师范大学 | Preparation method of water-soluble CdTe quantum dot |
| CN102786039A (en) * | 2012-08-30 | 2012-11-21 | 中国科学院长春应用化学研究所 | Preparation method of water soluble ZnSe quantum dots |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101870459A (en) * | 2010-06-11 | 2010-10-27 | 山东大学 | Method for preparing water-soluble CdTe quantum dots |
| CN102060273A (en) * | 2010-11-05 | 2011-05-18 | 桂林理工大学 | Method for preparing I-III-VI group semiconductor material through solvothermal synthesis in constant pressure open system |
| CN102634342A (en) * | 2012-03-31 | 2012-08-15 | 华东师范大学 | Preparation method of water-soluble CdTe quantum dot |
| CN102786039A (en) * | 2012-08-30 | 2012-11-21 | 中国科学院长春应用化学研究所 | Preparation method of water soluble ZnSe quantum dots |
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