CN101497787A - Method for synthesizing water-soluble blue luminescence quantum dot - Google Patents
Method for synthesizing water-soluble blue luminescence quantum dot Download PDFInfo
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- CN101497787A CN101497787A CNA2009101111212A CN200910111121A CN101497787A CN 101497787 A CN101497787 A CN 101497787A CN A2009101111212 A CNA2009101111212 A CN A2009101111212A CN 200910111121 A CN200910111121 A CN 200910111121A CN 101497787 A CN101497787 A CN 101497787A
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- halfcystine
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Abstract
The invention discloses a synthesis method of a simple and economic water soluble blue fluorescence quantum point, which adopts an environment-friendly mercapto compound, namely L-cysteine as stabilizing agent and uses cheap water without pollution as solvent to synthesize the blue fluorescence CdS quantum point by the pH control. The blue fluorescence quantum point prepared by the preparation method has uniform grain diameter distribution, high photochemistry stability and good reproduction quality, thereby providing a rapid, simple, economic and environment-friendly synthesis method for the preparation of the water soluble blue fluorescence quantum point with high quality, great market competitiveness and better application prospect.
Description
Technical field
The present invention relates to the synthetic method of fluorescence quantum, specifically is the synthetic method of water-soluble blue luminescence quantum dot.
Background technology
Fluorescence quantum has been widely used in field of electronic devices, but in the application of photodiode, blue luminescence quantum dot is optimal.Yet synthetic rare report about blue luminescence quantum dot, and the inherent valence band width of quantum dot defines its spectral range, the emmission spectrum of CdSe can cover whole visible region, particle diameter is blue less than the CdSe quantum dot fluorescence of 2nm, but the CdSe quantum point grain diameter of this small particle size disperses inhomogeneous and quantum yield is low.CdS can obtain stronger fluorescence in the blue-light-emitting zone, but synthesizing in organic phase of being reported carry out, and needs higher temperature of reaction, has caused synthetic difficulty bigger, and process is wayward.(CdS) the ZnS nuclear shell structure quantum point can obtain the emission wavelength of 468nm, but building-up process is to carry out in organic phase equally, and the application of gained quantum dot is very limited.
Summary of the invention
The purpose of this invention is to provide a kind of simple synthetic method of economic water-soluble blue luminescence quantum dot again.
Technical scheme of the present invention is such: the synthetic method of water-soluble blue luminescence quantum dot, realize as follows:
One, with the KBH of 0.1～0.3g
4Place colorimetric cylinder with the mixture of the Te powder of 0.1～0.3g, add 2～5mL ultrapure water, feed nitrogen 15～30min, place the frozen water territory to react 8～15h, make KHTe solution and store with standby;
Two, under the magnetic agitation with the CdCl of 0.4～1.0g
22.5H
2O is dissolved in 70～90ml ultrapure water, the L-halfcystine of 0.6～1.3g is dissolved in 15～25ml ultrapure water, the mol ratio of control Cd:L-halfcystine is 1:2～1:3, regulate pH value to 9.0～12.0 with 0.5～1mol/L NaOH solution, feed the high pure nitrogen deoxygenation, add above-mentioned KHTe solution under vigorous stirring rapidly, the mol ratio of control Te:Cd obtains quantum dot precursor solution at 1:1～1:2;
Three, with quantum dot precursor solution backflow 1～6h under 100～120 ℃, placed 2～7 days the cooling back, and pH is 1.0～4.0 with 1～3mol/L HCl adjusting gained quantum dot solution; Centrifugation, its supernatant liquor then are blue-fluorescence CdS quantum dot, and emission wavelength is at 432nm.
After adopting such scheme, beneficial effect of the present invention is: adopting environment-friendly type sulfhydryl compound L-halfcystine is stablizer, is solvent with water pollution-free and cheap and easy to get, has synthesized blue-fluorescence CdS quantum dot by the pH regulation and control.Prepared blue luminescence quantum dot size distribution is even, the photochemical stability height, favorable reproducibility, this preparation for water-soluble high-quality blue luminescence quantum dot provides one fast, simple, economy, environment-friendly type synthetic method, and product will have the strong market competitiveness and good prospects for application.
Embodiment
Embodiment one:
The synthetic method of water-soluble blue luminescence quantum dot of the present invention, realize as follows:
1, with 0.1079g KBH
4Place the 10mL colorimetric cylinder with the mixture of 0.1275g Te powder, add the 5mL ultrapure water, feed nitrogen 30min, place the frozen water territory to react 10h, make KHTe solution and store with standby;
2, under the magnetic agitation with the CdCl of 0.4567g
22.5H
2O is dissolved in the 80ml ultrapure water, the 0.608gL-halfcystine is dissolved in the 20mL ultrapure water, regulate pH value to 11.0 with 1mol/L NaOH solution, obtain the mixing solutions of halfcystine and Cadmium chloride fine powder, with high pure nitrogen the deoxidation in enclosed system of this mixing solutions is protected, under vigorous stirring, add above-mentioned KHTe solution rapidly, obtain quantum dot precursor solution;
3, with quantum dot precursor solution at 110 ℃ of following backflow 1h, placed 2 days cooling back, regulating gained quantum dot solution pH value with 1mol/LHCl is 1.3; Centrifugation, its supernatant liquor then are blue-fluorescence CdS quantum dot, and emission wavelength is at 432nm.
Embodiment two:
The synthetic method of water-soluble blue luminescence quantum dot of the present invention, realize as follows:
1, with 0.2158g KBH
4Place the 10mL colorimetric cylinder with the mixture of 0.2550g Te powder, add the 5mL ultrapure water, feed nitrogen 30min, place the frozen water territory to react 12h, make KHTe solution and store with standby;
2, under the magnetic agitation with the CdCl of 0.9134g
22.5H
2O is dissolved in the 90ml ultrapure water, the 1.212gL-halfcystine is dissolved in the 23mL ultrapure water, regulate pH value to 11.0 with 1mol/L NaOH solution, obtain the mixing solutions of halfcystine and Cadmium chloride fine powder, with high pure nitrogen the deoxidation in enclosed system of this mixing solutions is protected, under vigorous stirring, add above-mentioned KHTe solution rapidly, obtain quantum dot precursor solution;
3, with quantum dot precursor solution at 110 ℃ of following backflow 6h, placed 7 days cooling back, regulating gained quantum dot solution pH value with 1mol/LHCl is 3.3; Centrifugation, its supernatant liquor then are blue-fluorescence CdS quantum dot, and emission wavelength is at 432nm.
Embodiment three:
The synthetic method of water-soluble blue luminescence quantum dot of the present invention, realize as follows:
1, with 0.2158g KBH
4Place the 10mL colorimetric cylinder with the mixture of 0.2550g Te powder, add the 5mL ultrapure water, feed nitrogen 30min, place the frozen water territory to react 12h, make KHTe solution and store with standby;
2, under the magnetic agitation with the CdCl of 0.9134g
22.5H
2O is dissolved in the 80ml ultrapure water, the 1.216gL-halfcystine is dissolved in the 20mL ultrapure water, regulate pH value to 9.0 with 1mol/L NaOH solution, obtain the mixing solutions of halfcystine and Cadmium chloride fine powder, with high pure nitrogen the deoxidation in enclosed system of this mixing solutions is protected, under vigorous stirring, add above-mentioned KHTe solution rapidly, obtain quantum dot precursor solution;
3, with quantum dot precursor solution at 120 ℃ of following backflow 3h, placed 3 days cooling back, regulating gained quantum dot solution pH value with 1mol/LHCl is 2.6; Centrifugation, its supernatant liquor then are blue-fluorescence CdS quantum dot, and emission wavelength is at 432nm.
Claims (1)
1, the synthetic method of water-soluble blue luminescence quantum dot is characterized in that: realize as follows:
One, with the KBH of 0.1～0.3g
4Place colorimetric cylinder with the mixture of the Te powder of 0.1～0.3g, add 2～5mL ultrapure water, feed nitrogen 15～30min, place the frozen water territory to react 8～15h, make KHTe solution and store with standby;
Two, under the magnetic agitation with the CdCl of 0.4～1.0g
22.5H
2O is dissolved in 70～90ml ultrapure water, the L-halfcystine of 0.6～1.3g is dissolved in 15～25ml ultrapure water, the mol ratio of control Cd:L-halfcystine is 1:2～1:3, regulate pH value to 9.0～12.0 with 0.5～1mol/L NaOH solution, feed the high pure nitrogen deoxygenation, add above-mentioned KHTe solution under vigorous stirring rapidly, the mol ratio of control Te:Cd obtains quantum dot precursor solution at 1:1～1:2;
Three, with quantum dot precursor solution backflow 1～6h under 100～120 ℃, placed 2～7 days the cooling back, and pH is 1.0～4.0 with 1～3mol/L HCl adjusting gained quantum dot solution; Centrifugation, its supernatant liquor then are blue-fluorescence CdS quantum dot, and emission wavelength is at 432nm.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200910111121 CN101497787B (en) | 2009-02-24 | 2009-02-24 | Method for synthesizing water-soluble blue luminescence quantum dot |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200910111121 CN101497787B (en) | 2009-02-24 | 2009-02-24 | Method for synthesizing water-soluble blue luminescence quantum dot |
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| Publication Number | Publication Date |
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| CN101497787A true CN101497787A (en) | 2009-08-05 |
| CN101497787B CN101497787B (en) | 2013-04-10 |
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| CN 200910111121 Expired - Fee Related CN101497787B (en) | 2009-02-24 | 2009-02-24 | Method for synthesizing water-soluble blue luminescence quantum dot |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101891241A (en) * | 2010-07-07 | 2010-11-24 | 华侨大学 | Novel method for synthesizing water-soluble blue-fluorescence quantum points |
| CN101704507B (en) * | 2009-12-04 | 2012-07-04 | 华东师范大学 | Method for synthesizing quantum dot with core-shell-shell structure in aqueous phase |
| CN103316692A (en) * | 2013-06-24 | 2013-09-25 | 江苏大学 | Preparation method and application of CdS/CNTs composite photocatalyst |
| CN115124069A (en) * | 2022-04-22 | 2022-09-30 | 西咸新区青氢华屹能源科技有限公司 | Method for preparing hydrogen by catalyzing formic acid through quantum dots under visible light |
-
2009
- 2009-02-24 CN CN 200910111121 patent/CN101497787B/en not_active Expired - Fee Related
Non-Patent Citations (1)
| Title |
|---|
| 李珊珊等: "强发光的CdS量子点的水相制备及其表面修饰", 《东华大学学报(自然科学版)》 * |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101704507B (en) * | 2009-12-04 | 2012-07-04 | 华东师范大学 | Method for synthesizing quantum dot with core-shell-shell structure in aqueous phase |
| CN101891241A (en) * | 2010-07-07 | 2010-11-24 | 华侨大学 | Novel method for synthesizing water-soluble blue-fluorescence quantum points |
| CN103316692A (en) * | 2013-06-24 | 2013-09-25 | 江苏大学 | Preparation method and application of CdS/CNTs composite photocatalyst |
| CN115124069A (en) * | 2022-04-22 | 2022-09-30 | 西咸新区青氢华屹能源科技有限公司 | Method for preparing hydrogen by catalyzing formic acid through quantum dots under visible light |
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| CN101497787B (en) | 2013-04-10 |
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