CN101891241A - Novel method for synthesizing water-soluble blue-fluorescence quantum points - Google Patents
Novel method for synthesizing water-soluble blue-fluorescence quantum points Download PDFInfo
- Publication number
- CN101891241A CN101891241A CN 201010224087 CN201010224087A CN101891241A CN 101891241 A CN101891241 A CN 101891241A CN 201010224087 CN201010224087 CN 201010224087 CN 201010224087 A CN201010224087 A CN 201010224087A CN 101891241 A CN101891241 A CN 101891241A
- Authority
- CN
- China
- Prior art keywords
- solution
- water
- soluble blue
- fluorescence quantum
- value
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Abstract
The invention discloses a novel method for synthesizing water-soluble blue-fluorescence quantum points, which comprises the following steps: adding CdC12 . 2.5H2O into secondary cooling water and stirring in a container; adding L-Cysteine into the secondary cooling water; dissolving under the high-purity N2 deoxygenation protection; pouring into the container for reaction until the components are dissolved completely to obtain a lacte feculent solution; adjusting the pH value of the lacte feculent solution with NaOH or KOH to about 7 to clear the lacte feculent solution; continually adjusting the pH value of the solution to 9-10 with NaOH or KOH; and carrying out heating reflux on the solution for 1-6h, adjusting the pH value of the solution to be 1-3 with HCl, wherein the supernate of the solution is the water-soluble blue-fluorescence quantum point, and the emission wavelength is 430nm. The invention takes environment-friendly L-Cysteine as a monophyletic precursor which is not only a stabilizing agent but also a sulfur source, can obtain the water-soluble blue-fluorescence quantum points with excellent fluorescence property by adjusting the pH value. The method of the invention can not generate toxic substance in the process of synthesis, and can synthesize the water-soluble blue-fluorescence quantum points under the condition of water bath under normal pressure, and has simple operation and low cost.
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
Blue light has a very wide range of applications at aspects such as photoelectronics and optical storages, all is the field of paying close attention in the world, forward position all the time.Particularly in recent years, along with deepening continuously of semiconductor nanocrystal research, further developing of blue light source obtained new opportunity.The semiconductor nanocrystal quantum dot is an important component part of nano material, have many good optical properties such as good light stability, fluorescence intensity height, demonstrate remarkable advantages in research fields such as opto-electronic device and biomedicines, caused people's concern more and more widely.
In the nanocrystalline bibliographical information of the CdS of some synthesizing water-solubilities, its precursor is Cd (ClO
4)
2, and the sulphur precursor is thiocarbamide or hydrogen sulfide, and part is some water miscible mercaptan, and as thioglycerol etc., thiocarbamide can discharge toxic substance H under the condition of heating
2S.
Summary of the invention
The novel method that the purpose of this invention is to provide a kind of synthesizing water-soluble blue-fluorescence quantum points, it can not produce toxic substance in building-up process, and gets final product synthesizing water-soluble blue-fluorescence quantum points CdS under the normal pressure water bath condition, and simple to operate, cost is low.
Technical scheme of the present invention is such: the novel method of synthesizing water-soluble blue-fluorescence quantum points is achieved by the following scheme: with the CdCl of 4-12mmol
22.5H
2O is loaded in the container, adds 140ml secondary water and stirs; The L-halfcystine of 10-30mmol is put into 60ml secondary water, in high-purity N
2Dissolve under the deoxidation protection; pour in the said vesse after treating to dissolve fully and react; obtain the oyster white turbid solution; NaOH or KOH with 1-3mol/L transfers about pH to 7 with this oyster white turbid solution; make the oyster white turbid solution become clarification; continue to transfer pH to 9-10 with NaOH or the KOH of 1-3mol/L; again this solution is carried out reflux 1-6h; transfer the pH to 1-3 of this solution with the HCl of 6-8mol/L; the supernatant liquor of this solution is water-soluble blue luminescence quantum dot, and emission wavelength is at 430nm.
The applicant finds, the precursor thiocarbamide of sulphur is nanocrystalline optional for synthetic CdS, water miscible L-halfcystine also can discharge the sulphur negative ion under the condition of alkalescence heating, water miscible like this L-halfcystine can discharge the sulphur negative ion as the sulphur source, and it is nanocrystalline simultaneously also to coat the water miscible CdS of synthetic as part.Because when heating, the speed that water soluble L-cysteine discharges the sulphur negative ion is very slow.Therefore, the nanocrystalline nucleation and growth speed of CdS is also very slow, thereby we can control nanocrystalline size by the reaction times.
After adopting such scheme, the novel method of synthesizing water-soluble blue-fluorescence quantum points of the present invention, L-halfcystine with environment-friendly type is a single-source precursor, it both had been a stablizer, it also is the sulphur source, by the regulation and control of pH value, can obtain photoluminescent property good water-solubility blue-fluorescence (synthetic emission peak positions is at 430nm) quantum dot.The inventive method can not produce toxic substance in building-up process, and can synthesize under the normal pressure water bath condition, and simple to operate, cost is low.
Embodiment
Embodiment one:
The novel method of synthesizing water-soluble blue-fluorescence quantum points of the present invention is achieved by the following scheme:
Take by weighing the CdCl of 4mmol
22.5H
2O puts into the beaker of 250ml, adds 140ml secondary water in this beaker, stirs down in magnetic stirring apparatus; Claim the L-halfcystine of 10mmol to put into 60ml secondary water again, in high-purity N
2Deoxidation protection dissolving down; pour in the above-mentioned beaker after treating to dissolve fully and react; obtain the oyster white turbid solution; NaOH with 1mol/L transfers to this oyster white turbid solution pH value about 7; make this oyster white turbid solution become clarification; continue the pH value of solution to be transferred to 9 with the NaOH of 1mol/L; obtain the quantum dot presoma; this solution is transferred to reflux 2h in the 250ml three-necked bottle; HCl with 6mol/L transfers pH value of solution=1.5; the supernatant liquor of this solution is water-soluble blue luminescence quantum dot, and emission wavelength is at 430nm.
Embodiment two:
The novel method of synthesizing water-soluble blue-fluorescence quantum points of the present invention is achieved by the following scheme: the CdCl that takes by weighing 8mmol
22.5H
2O puts into the beaker of 250ml, adds 140ml secondary water in this beaker, stirs down in magnetic stirring apparatus; Claim the L-halfcystine of 20mmol to put into 60ml secondary water again, in high-purity N
2Deoxidation protection dissolving down; pour in the above-mentioned beaker after treating to dissolve fully and react; obtain the oyster white turbid solution; KOH with 1mol/L transfers to this oyster white turbid solution pH value about 7; make this oyster white turbid solution become clarification; continue the pH value of solution to be transferred to 10 with the KOH of 1mol/L; obtain the quantum dot presoma; this solution is transferred to reflux 2h in the 250ml three-necked bottle; HCl with 6mol/L transfers pH value of solution=1.5; the supernatant liquor of this solution is water-soluble blue luminescence quantum dot, and emission wavelength is at 430nm.
Embodiment three:
The novel method of synthesizing water-soluble blue-fluorescence quantum points of the present invention is achieved by the following scheme: the CdCl that takes by weighing 12mmol
22.5H
2O puts into the beaker of 250ml, adds 140ml secondary water in this beaker, stirs down in magnetic stirring apparatus; Claim the L-halfcystine of 20mmol to put into 60ml secondary water again, in high-purity N
2Deoxidation protection dissolving down; pour in the above-mentioned beaker after treating to dissolve fully and react; obtain the oyster white turbid solution; NaOH with 1mol/L transfers to this oyster white turbid solution pH value about 7; make this oyster white turbid solution become clarification; continue the pH value of solution to be transferred to 10 with the NaOH of 1mol/L; obtain the quantum dot presoma; this solution is transferred to reflux 2h in the 250ml three-necked bottle; HCl with 8mol/L transfers pH value of solution=1.5; the supernatant liquor of this solution is water-soluble blue luminescence quantum dot, and emission wavelength is at 430nm.
Claims (1)
1. the novel method of synthesizing water-soluble blue-fluorescence quantum points is characterized in that: be achieved by the following scheme: with the CdCl of 4-12mmol
22.5H
2O is loaded in the container, adds 140ml secondary water and stirs; The L-halfcystine of 10-30mmol is put into 60ml secondary water, in high-purity N
2Dissolve under the deoxidation protection; pour in the said vesse after treating to dissolve fully and react; obtain the oyster white turbid solution; NaOH or KOH with 1-3mol/L transfers about pH to 7 with this oyster white turbid solution; make the oyster white turbid solution become clarification; continue to transfer pH to 9-10 with NaOH or the KOH of 1-3mol/L; again this solution is carried out reflux 1-6h; transfer the pH to 1-3 of this solution with the HCl of 6-8mol/L; the supernatant liquor of this solution is water-soluble blue luminescence quantum dot, and emission wavelength is at 430nm.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 201010224087 CN101891241A (en) | 2010-07-07 | 2010-07-07 | Novel method for synthesizing water-soluble blue-fluorescence quantum points |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 201010224087 CN101891241A (en) | 2010-07-07 | 2010-07-07 | Novel method for synthesizing water-soluble blue-fluorescence quantum points |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN101891241A true CN101891241A (en) | 2010-11-24 |
Family
ID=43100620
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 201010224087 Pending CN101891241A (en) | 2010-07-07 | 2010-07-07 | Novel method for synthesizing water-soluble blue-fluorescence quantum points |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN101891241A (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102660258A (en) * | 2012-04-18 | 2012-09-12 | 中国科学院化学研究所 | Method for preparing water-soluble CdS quantum dot |
| 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 |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1952038A (en) * | 2005-10-21 | 2007-04-25 | 中国科学院上海应用物理研究所 | Cadmium sulfide bare quantum spot and preparation process |
| WO2008140495A2 (en) * | 2006-11-22 | 2008-11-20 | The Research Foundation Of State University Of New York | A method to produce water-dispersible highly luminescent quantum dots for biomedical imaging |
| CN101497787A (en) * | 2009-02-24 | 2009-08-05 | 华侨大学 | Method for synthesizing water-soluble blue luminescence quantum dot |
| CN101638579A (en) * | 2009-08-21 | 2010-02-03 | 天津城市建设学院 | Quantum dot-cyanine dye-folic acid biological probe and preparation method thereof |
| CN101704516A (en) * | 2009-11-27 | 2010-05-12 | 华东师范大学 | Method for synthesizing quantum dot with uniform size distribution in aqueous phase |
-
2010
- 2010-07-07 CN CN 201010224087 patent/CN101891241A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1952038A (en) * | 2005-10-21 | 2007-04-25 | 中国科学院上海应用物理研究所 | Cadmium sulfide bare quantum spot and preparation process |
| WO2008140495A2 (en) * | 2006-11-22 | 2008-11-20 | The Research Foundation Of State University Of New York | A method to produce water-dispersible highly luminescent quantum dots for biomedical imaging |
| CN101497787A (en) * | 2009-02-24 | 2009-08-05 | 华侨大学 | Method for synthesizing water-soluble blue luminescence quantum dot |
| CN101638579A (en) * | 2009-08-21 | 2010-02-03 | 天津城市建设学院 | Quantum dot-cyanine dye-folic acid biological probe and preparation method thereof |
| CN101704516A (en) * | 2009-11-27 | 2010-05-12 | 华东师范大学 | Method for synthesizing quantum dot with uniform size distribution in aqueous phase |
Non-Patent Citations (1)
| Title |
|---|
| 《安徽农业科学》 20091231 郭伟等 水溶性L-Cys-CdS量子点与牛血清白蛋白相互作用研究 16230-16239 1 第37卷, 第33期 2 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102660258A (en) * | 2012-04-18 | 2012-09-12 | 中国科学院化学研究所 | Method for preparing water-soluble CdS quantum dot |
| 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 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| Ni et al. | Hydrothermal preparation and optical properties of ZnO nanorods | |
| CN104498039B (en) | A kind of acid auxiliary prepares the synthetic method of CdSe/CdS/ZnS nuclear shell structure quantum point | |
| CN100572500C (en) | The aqueous phase preparation method of cyclodextrin modified CdTe quantum dot | |
| CN101891241A (en) | Novel method for synthesizing water-soluble blue-fluorescence quantum points | |
| TW200642963A (en) | Surface modified nanoparticle and method of preparing same | |
| CN102826585A (en) | Method for producing ultra-small water soluble near-infrared Ag2S quantum dots | |
| CN110734767A (en) | method for preparing size-controllable organic phase silver selenide quantum dots | |
| Li et al. | A review on the synthesis methods of CdSeS-based nanostructures | |
| CN104877685B (en) | Preparation method of ZnSe/ ZnS quantum dot for core-shell structure of photoelectric device | |
| CN100494309C (en) | Synthesis method of core/shell type cadmium telluride/cadmium sulfide water-soluble quantum dot | |
| CN103436256A (en) | Aqueous-phase synthesis method of Cu-doped Zn1-xCdxS quantum dot and core/shell structure thereof | |
| Wang et al. | One-pot synthesis of CdSe quantum dots using selenium dioxide as a selenium source in aqueous solution | |
| CN101798511A (en) | Method for preparing group II-VI soluble selenide semiconductor quantum dots by gas phase method | |
| CN103539082B (en) | Quick green preparation method of cadmium telluride quantum dot | |
| CN102086397A (en) | Method for fast preparing soluble near infrared CdTe quantum dots covered with mercaptan in aqueous phase | |
| CN107858145A (en) | quantum dot and its synthetic method | |
| CN105838357A (en) | Preparation method of zinc and silver co-doped cadmium sulfide quantum dots | |
| Liu et al. | Aqueous synthesis of thiol-capped CdTe quantum dots and its photoluminescence enhancement via room temperature treatment with alkyl chain diamines | |
| Yu et al. | Effect of ligands on the photoluminescence properties of water-soluble PbS quantum dots | |
| CN105505393A (en) | Method for rapidly and remarkably enhancing fluorescence intensity of quantum dots | |
| Kumar et al. | Optical properties of colloidal aqueous synthesized 3 mercaptopropionic acid stabilized CdS quantum dots | |
| CN103992797A (en) | Method for surface modification of ZnSe:Ag quantum dots | |
| Gao et al. | Synthesis of highly emissive CdSe quantum dots by aqueous precipitation method | |
| Zhou et al. | One-pot aqueous phase synthesis of CdTe and CdTe/ZnS core/Shell quantum dots | |
| CN104403670B (en) | A kind of preparation method of cadmium, ytterbium codope ZnS quantum dots |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C12 | Rejection of a patent application after its publication | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20101124 |