CN105838358B - A kind of Er ions ZnxCd1-xThe microwave preparation of S quantum dots - Google Patents
A kind of Er ions ZnxCd1-xThe microwave preparation of S quantum dots Download PDFInfo
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- CN105838358B CN105838358B CN201410802630.0A CN201410802630A CN105838358B CN 105838358 B CN105838358 B CN 105838358B CN 201410802630 A CN201410802630 A CN 201410802630A CN 105838358 B CN105838358 B CN 105838358B
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Abstract
The present invention relates to a kind of Er ions ZnxCd1‑xThe microwave preparation of S quantum dots.It is primarily characterized in that：With Zn (CH3COO)2·2H2O is zinc source, with CdCl2·2.5H2O is cadmium source, with Er (NO3)3·5H2O is erbium source, is made into mixed solution, under nitrogen protection, uses glutathione（GSH）Make stabilizer, in alkaline aqueous solution, Na is added2S·9H2O solution, microwave heating obtain Er ions ZnxCd1‑xS quantum dots.Low energy consumption for the microwave the preparation method, simple for process and environmentally protective, gained quantum dot uniform particle sizes, it is water-soluble good, fluorescence and chemical property are good, by changing doping ratio, the adjustable fluorescent emission peak position such as reaction temperature, can be widely applied to fluorescence probe, drug screening and environmental monitoring etc..
Description
Technical field
The present invention relates to a kind of preparing technical field of novel fluorescence nano material, more particularly to a kind of Er ions
ZnxCd1-xThe microwave preparation of S quantum dots.
Background technology
ZnS quantum dot is a kind of important semi-conducting material of II-VI races, has high projection and folding in visible-range
Coefficient is penetrated, there are excellent fluorescent effect and photoelectric effect and the advantages such as high stability, low cost, nontoxic.ZnS is broadband
Gap luminescent material after doped metal ion, can adjust its bandwidth, to regulate and control fluorescence emission wavelengths, improve its fluorescence
Efficiency and stability.
The preparation method of ZnS quantum dots mainly use organic synthesis method, this method severe reaction conditions, expensive reagents,
The shortcomings of raw material is toxic；The microwave-hydrothermal method of use is a kind of easy to operate, and low energy consumption, environmentally protective synthetic method；In table
Using the surface of nontoxic glutathione modification quantum dot on the dressing agent of face, avoid using other toxic stabilizers.
Invention content
The purpose of the present invention is to provide a kind of Er ions ZnxCd1-xThe microwave preparation of S quantum dots.The quantum dot
Uniform particle sizes have excellent water solubility and fluorescence.
The technical solution adopted by the present invention is：
A kind of Er ions Zn of the present inventionxCd1-xThe molar ratio of S quantum dots, erbium ion and zinc ion is 0.01:1 ~
0.08:1, the molar ratio of cadmium ion and zinc ion is 0.1:1 ~ 0.8:1;.
The preparation method of a kind of cerium, erbium-codoped ZnS quantum dot, is as follows：
（1）By the Zn (CH of certain mol proportion example3COO)2·2H2O、CdCl2·2.5H2O、Er(NO3)3·5H2O is added suitable
In the deionized water of amount, stir evenly；
（2）By glutathione（GSH）、NaOH、Na2S·9H2O is dissolved separately in suitable deionized water, is made into corresponding
GSH solution, NaOH solution, the Na of concentration2S·9H2O solution；
(3) under nitrogen protection, GSH solution is added dropwise to step（1）In solution, stir evenly；
（4）With NaOH solution regulating step（3）The pH value of solution；It is slowly added to Na2S·9H2O solution, stirs evenly；
（5）By step（4）Solution heating water bath under microwave, that is, arrive Er ions ZnxCd1-xS quantum dot aqueous solutions；
（6）Step（5）After solution cooling, the absolute ethyl alcohol of equivalent is added, precipitation is precipitated, centrifuges, uses absolute ethyl alcohol
Cleaning precipitation, vacuum drying obtain Er ions ZnxCd1-xS quantum dots.
Main advantages of the present invention are：With microwave Aqueous phase synthesis Er ions ZnxCd1-xS quantum dots, the preparation method institute
Advantages of nontoxic raw materials, simple for process and environmentally protective, low energy consumption；Gained quantum dot uniform particle sizes, excellent water-solubility, fluorescent stabilization
Property it is good, by change Doped ions ratio, reaction temperature etc., fluorescent emission peak position can be adjusted in the nm of 436 nm ~ 525
Between.
Specific implementation mode
In order to which the features of the present invention is described in more detail, the present invention is made below by specific embodiment further
It illustrates, rather than limits the scope of the invention.
Embodiment 1：
By the Zn (CH that 30 mL molar concentrations are 0.05 mol/L3COO)2·2H2O and 10 ml molar concentrations are 0.05
The CdCl of mol/L2·2.5H2O solution is placed in a three-necked flask, and the Er that 3 mL molar concentrations are 0.01 mol/L is added
(NO3)3·5H2O solution, magnetic agitation are uniform；It is passed through high pure nitrogen half an hour, is 0.1 mol/L's by 18 mL molar concentrations
Glutathione（GSH）Solution is added drop-wise in above-mentioned solution, and magnetic agitation is uniform；
Under nitrogen protection, it is 12 to adjust above-mentioned solution ph with NaOH solution, and magnetic agitation is uniform；It is slowly added to 16
The Na of a concentration of 0.1 mol/L of mL2S·9H2O solution continues to stir half an hour；Microwave heated aqueous, 90 DEG C of reaction temperature, instead
It is 15 minutes between seasonable, obtains Er ions ZnxCd1-xS quantum dot aqueous solutions.After solution cooling, the absolute ethyl alcohol of equivalent is added,
White precipitate is precipitated, centrifuges, with washes of absolute alcohol sediment, vacuum drying obtains Er ions ZnxCd1-xS quantum dots.
Embodiment 2：
By the Zn (CH that 50 mL molar concentrations are 0.05 mol/L3COO)2·2H2O and 30 ml molar concentrations are 0.05
The CdCl of mol/L2·2.5H2O solution is placed in a three-necked flask, and the Er that 5 mL molar concentrations are 0.01 mol/L is added
(NO3)3·5H2O solution, magnetic agitation are uniform；It is passed through high pure nitrogen half an hour, is 0.1 mol/L's by 22 mL molar concentrations
Glutathione（GSH）Solution is added drop-wise in above-mentioned solution, and magnetic agitation is uniform；
Under nitrogen protection, it is 8 to adjust above-mentioned solution ph with NaOH solution, and magnetic agitation is uniform；It is slowly added to 25 mL
The Na of a concentration of 0.1 mol/L2S·9H2O solution continues to stir half an hour；Microwave heated aqueous, 80 DEG C of reaction temperature, reaction
Time is 25 minutes, obtains Er ions ZnxCd1-xS quantum dot aqueous solutions.After solution cooling, the absolute ethyl alcohol of equivalent is added, analyses
Go out white precipitate, centrifuge, with washes of absolute alcohol sediment, vacuum drying obtains Er ions ZnxCd1-xS quantum dots.
Embodiment 3：
By the Zn (CH that 20 mL molar concentrations are 0.05 mol/L3COO)2·2H2O and 20 ml molar concentrations are 0.03
The CdCl of mol/L2·2.5H2O solution is placed in a three-necked flask, and the Er that 3 mL molar concentrations are 0.01 mol/L is added
(NO3)3·5H2O solution, magnetic agitation are uniform；It is passed through high pure nitrogen half an hour, is 0.1 mol/L's by 10 mL molar concentrations
Glutathione（GSH）Solution is added drop-wise in above-mentioned solution, and magnetic agitation is uniform；
Under nitrogen protection, it is 9 to adjust above-mentioned solution ph with NaOH solution, and magnetic agitation is uniform；It is slowly added to 11 mL
The Na of a concentration of 0.1 mol/L2S·9H2O solution continues to stir half an hour；Microwave heated aqueous, 90 DEG C of reaction temperature, reaction
Time is 10 minutes, obtains Er ions ZnxCd1-xS quantum dot aqueous solutions.After solution cooling, the absolute ethyl alcohol of equivalent is added, analyses
Go out white precipitate, centrifuge, with washes of absolute alcohol sediment, vacuum drying obtains Er ions ZnxCd1-xS quantum dots.
Embodiment 4：
By the Zn (CH that 30 mL molar concentrations are 0.1 mol/L3COO)2·2H2O and 20 ml molar concentrations are 0.1
The CdCl of mol/L2·2.5H2O solution is placed in a three-necked flask, and the Er that 3 mL molar concentrations are 0.05 mol/L is added
(NO3)3·5H2O solution, magnetic agitation are uniform；It is passed through high pure nitrogen half an hour, is 0.1 mol/L's by 28 mL molar concentrations
Glutathione（GSH）Solution is added drop-wise in above-mentioned solution, and magnetic agitation is uniform；
Under nitrogen protection, it is 11.5 to adjust above-mentioned solution ph with NaOH solution, and magnetic agitation is uniform；It is slowly added to 30
The Na of a concentration of 0.1 mol/L of mL2S·9H2O solution continues to stir half an hour；Microwave heated aqueous, 70 DEG C of reaction temperature, instead
It is 35 minutes between seasonable, obtains Er ions ZnxCd1-xS quantum dot aqueous solutions.After solution cooling, the absolute ethyl alcohol of equivalent is added,
White precipitate is precipitated, centrifuges, with washes of absolute alcohol sediment, vacuum drying obtains Er ions ZnxCd1-xS quantum dots.
Claims (1)
1. a kind of Er ions ZnxCd1-xThe microwave preparation of S quantum dots, it is characterised in that：
（1）By the Zn (CH of certain mol proportion example3COO)2·2H2O、CdCl2·2.5H2O、Er(NO3)3·5H2O is added suitable
In deionized water, stir evenly；
（2）By glutathione（GSH）、NaOH、Na2S·9H2O is dissolved separately in suitable deionized water, is made into respective concentration
GSH solution, NaOH solution, Na2S·9H2O solution；
(3) under nitrogen protection, GSH solution is added dropwise to step（1）In solution, stir evenly；
（4）With NaOH solution regulating step（3）The pH value of solution；It is slowly added to Na2S·9H2O solution, stirs evenly；
（5）By step（4）Solution heating water bath under microwave, obtains Er ions ZnxCd1-xS quantum dot aqueous solutions；
（6）Step（5）After solution cooling, the absolute ethyl alcohol of equivalent is added, precipitation is precipitated, centrifuges, uses washes of absolute alcohol
Precipitation, vacuum drying obtain Er ions ZnxCd1-xS quantum dots.
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101824317A (en) * | 2010-04-28 | 2010-09-08 | 天津大学 | CdxZn1-xS/ZnS ternary core-shell quantum dot and method for preparing same |
| EP2184333B1 (en) * | 2008-11-05 | 2013-07-17 | Samsung Electronics Co., Ltd. | Quantum dot electroluminescent device and method for fabricating the same |
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| KR100678285B1 (en) * | 2005-01-20 | 2007-02-02 | 삼성전자주식회사 | Quantum Dot Phosphor for Light Emitting Diode and Method of Preparing Thereof |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP2184333B1 (en) * | 2008-11-05 | 2013-07-17 | Samsung Electronics Co., Ltd. | Quantum dot electroluminescent device and method for fabricating the same |
| CN101824317A (en) * | 2010-04-28 | 2010-09-08 | 天津大学 | CdxZn1-xS/ZnS ternary core-shell quantum dot and method for preparing same |
Non-Patent Citations (3)
| Title |
|---|
| CdxZn1-xS:SmF3的红色薄膜电致发光;朱佳等;《发光学报》;19911231;第12卷(第4期);285-290 * |
| Cd掺杂ZnS量子点的光学性能研究;胡智学等;《分析科学学报》;20131231;753-757 * |
| Er 离子掺杂 ZnS 量子点的水相法合成及性能;李丽华等;《河南科技大学学报:自然科学版》;20131031;5-9 * |
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