CN1974720A - Core-sheel structure M(1-x)Y2S4:Ax/ZnS quantum dot and its prepn process - Google Patents
Core-sheel structure M(1-x)Y2S4:Ax/ZnS quantum dot and its prepn process Download PDFInfo
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- CN1974720A CN1974720A CN 200610130073 CN200610130073A CN1974720A CN 1974720 A CN1974720 A CN 1974720A CN 200610130073 CN200610130073 CN 200610130073 CN 200610130073 A CN200610130073 A CN 200610130073A CN 1974720 A CN1974720 A CN 1974720A
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Abstract
The present invention discloses one kind of core-shell structure quantum dot with ZnS shell, and features its chemical expression of M(1-x)Y2S4 to Ax/ZnS, where, M is Bioavailability or Ca, A is one or two of Mn, Cu, Ag, Al, Pr, Eu, Er, Tm, Ce, Yb and Nd, x is 0.001-0.5. The present invention also provides the preparation process of the quantum dot. The preparation process has safe material, low material cost, simple and safe operation and relaxed equipment requirement, and is suitable for large scale preparation in lab. The prepared quantum dot has high dispersivity, high fluorescence strength and high stability, and may be used as fluorescent labeling material for biological detection and analysis and as light emitting material for display devices.
Description
[technical field]
The present invention relates to nano semiconductor material, especially a kind of M
(1-x)Y
2S
4: A
x/ ZnS core/shell structure quantum dot and preparation method thereof.
[background technology]
Quantum dot is accurate zero-dimension nano semiconductor material, and it is made of a small amount of atom or atomic group, and three dimension scale is at 1～10nm usually.Because the influence of size quantum effect and dielectric confinement effect, semiconductor nanocrystal demonstrate unique physics and chemical propertys such as fluorescent characteristic.Make quantum dot have broad application prospects at aspects such as optics and biology.Quantum dot has huge demand in life science and other fields, so people have also carried out constantly exploring for quantum dot and synthetic technology thereof.The nano particle that has synthesized at present multiple nucleocapsid structure, as: CdS/Ag
2S, CdS/Cd (OH)
2, CdS/ZnS, CdSe/ZnS, CdHgTe/ZnS, ZnSe/CdSe, CdS/HgS, CdS/PbS and multilayered structure CdS/HgS/CdS or the like.But face some problems too, the quanta point material that uses mostly is and contains Se at present, Cd, and the Te composition, its toxicity is bigger, the feedstock property instability, cost is very high, has greatly limited the preparation and the application thereof of quantum dot.By containing transition metal or rare earth ion in the matrix quanta point material, can solve quantum dot physical properties and spectrum demand and be difficult to unified problem, in the realization a plurality of wavelength band such as infrared fluorescent emission.Therefore, the doping type quantum dot that processability is good becomes an important directions of research.Simultaneously, because there are a large amount of defectives on the quantum dot surface of preparation usually, influence quantum yield.Take to coat the semiconductor material that another kind of crystalline structure is similar, band gap is bigger on the quantum dot surface, make the core/shell structure quantum dot, can strengthen its stability, and be a surperficial radiationless recombinable site quilt change, excite defective to improve its fluorescent characteristic greatly thereby reduce.
[summary of the invention]
The objective of the invention is in order to overcome the deficiencies in the prior art, and provide a kind of luminescent properties good quantum dot, and the preparation method of this quantum dot.
The present invention discloses a kind of M for addressing the above problem
(1-x)Y
2S
4: A
x/ ZnS core/shell structure quantum dot is characterized in that quantum dot is with M
(1-x)Y
2S
4: A
xFor nuclear, be shell with ZnS, its chemical expression is:
M
(1-x)Y
2S
4:A
x/ZnS
Wherein, M is a kind of element among Ba or the Ca; A is Mn, Cu, Ag, Al, Pr, Eu, Er, Tm, Ce, a kind of element among Yb or the Nd or the wherein mixing of two kinds of elements; 0.001＜x≤0.5.
The present invention also provides a kind of M
(1-x)Y
2S
4: A
x/ ZnS core/shell structure quantum dot preparation method, preparation method of the present invention may further comprise the steps:
1) according to stoichiometric ratio with in the water-soluble solution of the soluble salt of barium or calcium, adding 1-100ml concentration is the sodium hexametaphosphate solution of 0.15g/ml, stirs, and makes storing solution A;
2) according to stoichiometric ratio with in the water-soluble solution of the soluble salt of yttrium, ultra-sonic dispersion 10-100min makes storing solution B;
3) according to stoichiometric ratio with in the water-soluble solution of the soluble salt of dopant ion, ultra-sonic dispersion 10-100min makes storing solution C;
4) according to stoichiometric ratio sodium sulphite is dissolved in the ethanolic soln, ultra-sonic dispersion 10-100min makes storing solution D;
5) according to stoichiometric ratio with in the water-soluble solution of zinc acetate, ultra-sonic dispersion 10-100min makes storing solution E;
6) will with the water-soluble solution of sodium sulphite of mol ratios such as zinc acetate in, ultra-sonic dispersion 10-90min makes storing solution F;
7) storing solution A, storing solution B and storing solution C are moved in the three-necked bottle, feed nitrogen, storing solution D is moved in the constant pressure funnel the airtight back of reactor magnetic stirrer solution, splash into equably in the reactor of stirring, 0.5-3h back stopped reaction, supernatant liquor is removed in centrifugation;
8) with in the water-soluble and alcohol mixeding liquid of product, move in the three-necked bottle with storing solution E, feed nitrogen with the airtight back of reactor magnetic stirrer solution, storing solution F is moved in the constant pressure funnel, splash into equably in the reactor of stirring, 0.5-5h back stopped reaction, centrifugation, remove supernatant liquor,, use absolute ethanol washing three times again with microwave heating 1-8 minute with deionized water wash three times, with twice of deionized water wash, use absolute ethanol washing twice again, product is dissolved in dehydrated alcohol, obtain M
(1-x)Y
2S
4: A
x/ ZnS core/shell structure quantum dot.
The present invention has prepared M with soluble salt under the condition of room temperature, safety
(1-x)Y
2S
4: A
x/ ZnS core/shell structure quantum dot.The quantum dot materials safety of the present invention's preparation is easy to get, and is cheap, and simple and safe operation does not need harsh appointed condition, makes the laboratory mass preparation become possibility.With the quantum dot good dispersity that present method obtains, fluorescence intensity height, good stability.This quantum dot can be used as the fluorescent mark material, is widely used in biological detection and analysis, and is used for multiple display device as luminescent material.
[embodiment]
The invention provides a kind of ZnS is the core/shell structure quantum dot of shell, and its chemical expression is:
M
(1-x)Y
2S
4:A
x/ZnS
Wherein, M is Ba, and a kind of element among the Ca, A are Mn, Cu, Ag, Al, Pr, Eu, Er, Tm, Ce, Yb, a kind of element among the Nd or the wherein mixing of two kinds of elements, 0.001＜x≤0.5.
At this quantum dot M
(1-x)Y
2S
4: A
xIn the chemical expression of/ZnS, the numerical value of x also can be following scope:
0.1＜x≤0.5。
Reasonable quantum dot can be expressed as with following chemical expression:
(1)Ca
0.9Y
2S
4:Er
0.1/ZnS；
(2)Ba
0.96Y
2S
4:Mn
0.04/ZnS。
In addition, the data that can also press in the tabulation at the specific embodiment of core/shell structure quantum dot are determined:
| M | A | X | |
| 1 | Ba | Eu | 0.1 |
| 2 | Ba | Ag | 0.05 |
| 3 | Ba | Cu | 0.08 |
| 4 | Ba | Mn | 0.1 |
| 5 | Ba | Pr | 0.05 |
| 6 | Ca | Yb | 0.15 |
| 7 | Ca | Er | 0.1 |
| 8 | Ca | Ce | 0.21 |
| 9 | Ca | Mn | 0.09 |
| 10 | Ca | Eu | 0.05 |
The preparation of quantum dot of the present invention:
Embodiment one:
With Ca
0.9Y
2S
4: Er
0.1/ ZnS core/shell structure quantum dot is an example, and 0.0045mol calcium chloride is dissolved in the 10ml aqueous solution, and adding 40ml concentration is the sodium hexametaphosphate solution of 0.15g/ml, stirs, and makes storing solution A;
2) the 0.01mol Yttrium trinitrate is dissolved in the 30ml aqueous solution, ultra-sonic dispersion 30min makes storing solution B;
3) 0.0005mol acetic acid erbium is dissolved in the 10ml aqueous solution, ultra-sonic dispersion 30min makes storing solution C;
4) 0.02mol sodium sulphite is dissolved in the 10ml ethanolic soln, ultra-sonic dispersion 30min makes storing solution D;
5) the 0.01mol zinc acetate is dissolved in the 20ml aqueous solution, ultra-sonic dispersion 30min makes storing solution E;
6) 0.01mol sodium sulphite is dissolved in the 20ml aqueous solution, ultra-sonic dispersion 30min makes storing solution F;
7) storing solution A, storing solution B and storing solution C are moved in the three-necked bottle, feed nitrogen with the airtight back of reactor magnetic stirrer solution, storing solution D is moved in the constant pressure funnel, speed with 0.7mL/min, splash into equably in the reactor of stirring, stopped reaction behind the 2h, supernatant liquor is removed in centrifugation;
8) with in the water-soluble and alcohol mixeding liquid of product, move in the three-necked bottle with storing solution E, feed nitrogen with the airtight back of reactor magnetic stirrer solution, storing solution F is moved in the constant pressure funnel, speed with 0.7mL/min, splash into equably in the reactor of stirring, stopped reaction behind the 3h, supernatant liquor is removed in centrifugation, with deionized water wash three times, use absolute ethanol washing three times with microwave heating 4 minutes again,, use twice of absolute ethanol washing again with deionized water wash twice, the product that obtains is dissolved in the dehydrated alcohol, promptly obtains Ca
0.9Y
2S
4: Er
0.1/ ZnS core/shell structure quantum dot.
Embodiment two:
With Ca
0.95Y
2S
4: Eu
0.05/ ZnS core/shell structure quantum dot is an example, and 0.00475mol calcium chloride is dissolved in the 10ml aqueous solution, and adding 46ml concentration is the sodium hexametaphosphate solution of 0.15g/ml, stirs, and makes storing solution A;
2) the 0.01mol Yttrium trinitrate is dissolved in the 30ml aqueous solution, ultra-sonic dispersion 30min makes storing solution B;
3) 0.00025mol acetic acid europium is dissolved in the 10ml aqueous solution, ultra-sonic dispersion 30min makes storing solution C;
4) 0.02mol sodium sulphite is dissolved in the 10ml ethanolic soln, ultra-sonic dispersion 30min makes storing solution D;
5) the 0.01mol zinc acetate is dissolved in the 20ml aqueous solution, ultra-sonic dispersion 30min makes storing solution E;
6) 0.01mol sodium sulphite is dissolved in the 20ml aqueous solution, ultra-sonic dispersion 30min makes storing solution F;
7) storing solution A, storing solution B and storing solution C are moved in the three-necked bottle, feed nitrogen with the airtight back of reactor magnetic stirrer solution, storing solution D is moved in the constant pressure funnel, speed with 0.7mL/min, splash into equably in the reactor of stirring, stopped reaction behind the 2h, supernatant liquor is removed in centrifugation;
8) with in the water-soluble and alcohol mixeding liquid of product, move in the three-necked bottle with storing solution E, feed nitrogen with the airtight back of reactor magnetic stirrer solution, storing solution F is moved in the constant pressure funnel, speed with 0.7mL/min, splash into equably in the reactor of stirring, stopped reaction behind the 3h, supernatant liquor is removed in centrifugation, with deionized water wash three times, use absolute ethanol washing three times with microwave heating 4 minutes again,, use twice of absolute ethanol washing again with deionized water wash twice, the product that obtains is dissolved in the dehydrated alcohol, promptly obtains Ca
0.95Y
2S
4: Eu
0.05/ ZnS core/shell structure quantum dot.
Embodiment three:
With Ba
0.95Y
2S
4: Pr
0.05/ ZnS core/shell structure quantum dot is an example, and the 0.00475mol bariumchloride is dissolved in the 10ml aqueous solution, and adding 60ml concentration is the sodium hexametaphosphate solution of 0.15g/ml, stirs, and makes storing solution A;
2) the 0.01mol Yttrium trinitrate is dissolved in the 30ml aqueous solution, ultra-sonic dispersion 30min makes storing solution B;
3) the 0.00025mol praseodymium acetate is dissolved in the 10ml aqueous solution, ultra-sonic dispersion 30min makes storing solution C;
4) 0.02mol sodium sulphite is dissolved in the 10ml ethanolic soln, ultra-sonic dispersion 30min makes storing solution D;
5) the 0.01mol zinc acetate is dissolved in the 20ml aqueous solution, ultra-sonic dispersion 30min makes storing solution E;
6) 0.01mol sodium sulphite is dissolved in the 20ml aqueous solution, ultra-sonic dispersion 30min makes storing solution F;
7) storing solution A, storing solution B and storing solution C are moved in the three-necked bottle, feed nitrogen with the airtight back of reactor magnetic stirrer solution, storing solution D is moved in the constant pressure funnel, speed with 0.7mL/min, splash into equably in the reactor of stirring, stopped reaction behind the 2h, supernatant liquor is removed in centrifugation;
8) with in the water-soluble and alcohol mixeding liquid of product, move in the three-necked bottle with storing solution E, feed nitrogen with the airtight back of reactor magnetic stirrer solution, storing solution F is moved in the constant pressure funnel, speed with 0.7mL/min, splash into equably in the reactor of stirring, stopped reaction behind the 3h, supernatant liquor is removed in centrifugation, with deionized water wash three times, use absolute ethanol washing three times with microwave heating 5 minutes again,, use twice of absolute ethanol washing again with deionized water wash twice, the product that obtains is dissolved in the dehydrated alcohol, promptly obtains Ba
0.95Y
2S
4: Pr
0.05/ ZnS core/shell structure quantum dot.
Embodiment four:
With Ba
0.9Y
2S
4: Mn
0.1/ ZnS core/shell structure quantum dot is an example, and the 0.0045mol bariumchloride is dissolved in the 10ml aqueous solution, and adding 40ml concentration is the sodium hexametaphosphate solution of 0.15g/ml, stirs, and makes storing solution A;
2) the 0.01mol Yttrium trinitrate is dissolved in the 30ml aqueous solution, ultra-sonic dispersion 30min makes storing solution B;
3) the 0.0005mol manganese acetate is dissolved in the 10ml aqueous solution, ultra-sonic dispersion 30min makes storing solution C;
4) 0.02mol sodium sulphite is dissolved in the 10ml ethanolic soln, ultra-sonic dispersion 30min makes storing solution D;
5) the 0.01mol zinc acetate is dissolved in the 20ml aqueous solution, ultra-sonic dispersion 30min makes storing solution E;
6) 0.01mol sodium sulphite is dissolved in the 20ml aqueous solution, ultra-sonic dispersion 30min makes storing solution F;
7) storing solution A, storing solution B and storing solution C are moved in the three-necked bottle, feed nitrogen with the airtight back of reactor magnetic stirrer solution, storing solution D is moved in the constant pressure funnel, speed with 0.7mL/min, splash into equably in the reactor of stirring, stopped reaction behind the 2h, supernatant liquor is removed in centrifugation;
8) with in the water-soluble and alcohol mixeding liquid of product, move in the three-necked bottle with storing solution E, feed nitrogen with the airtight back of reactor magnetic stirrer solution, storing solution F is moved in the constant pressure funnel, speed with 0.7mL/min, splash into equably in the reactor of stirring, stopped reaction behind the 3h, supernatant liquor is removed in centrifugation, with deionized water wash three times, use absolute ethanol washing three times with microwave heating 6 minutes again,, use twice of absolute ethanol washing again with deionized water wash twice, the product that obtains is dissolved in the dehydrated alcohol, promptly obtains Ba
0.9Y
2S
4: Mn
0.1/ ZnS core/shell structure quantum dot.
Claims (5)
1, a kind of M
(1-x)Y
2S
4: A
x/ ZnS core/shell structure quantum dot is characterized in that quantum dot is with M
(1-x)Y
2S
4: A
xFor nuclear, be shell with ZnS, its chemical expression is:
M
(1-x)Y
2S
4:A
x/ZnS
Wherein, M is Ba, a kind of element among the Ca; A is Mn, Cu, Ag, Al, Pr, Eu, Er, Tm, Ce, Yb, a kind of element among the Nd or the wherein mixing of two kinds of elements; 0.001＜x≤0.5.
2, according to the described M of claim 1
(1-x)Y
2S
4: A
x/ ZnS core/shell structure quantum dot is characterized in that said
0.1＜x≤0.5。
3, according to claim 1 or 2 described M
(1-x)Y
2S
4: A
x/ ZnS core/shell structure quantum dot is characterized in that the chemical expression of said quantum dot is:
Ca
0.9Y
2S
4:Er
0.1/ZnS。
4, according to claim 1 or 2 described M
(1-x)Y
2S
4: A
x/ ZnS core/shell structure quantum dot is characterized in that the chemical expression of said quantum dot is:
Ba
0.96Y
2S
4:Mn
0.04/ZnS。
5, a kind of M of claim 1
(1-x)Y
2S
4: A
xThe preparation method of/ZnS core/shell structure quantum dot is characterized in that said preparation process is:
1) according to stoichiometric ratio with in the water-soluble solution of the soluble salt of barium or calcium, adding 1-100ml concentration is the sodium hexametaphosphate solution of 0.15g/ml, stirs, and makes storing solution A;
2) according to stoichiometric ratio with in the water-soluble solution of the soluble salt of yttrium, ultra-sonic dispersion 10-100min makes storing solution B;
3) according to stoichiometric ratio with in the water-soluble solution of the soluble salt of dopant ion, ultra-sonic dispersion 10-100min makes storing solution C;
4) according to stoichiometric ratio sodium sulphite is dissolved in the ethanolic soln, ultra-sonic dispersion 10-100min makes storing solution D;
5) according to stoichiometric ratio with in the water-soluble solution of zinc acetate, ultra-sonic dispersion 10-100min makes storing solution E;
6) will with the water-soluble solution of sodium sulphite of mol ratios such as zinc acetate in, ultra-sonic dispersion 10-90min makes storing solution F;
7) storing solution A, storing solution B and storing solution C are moved in the three-necked bottle, feed nitrogen, storing solution D is moved in the constant pressure funnel the airtight back of reactor magnetic stirrer solution, splash into equably in the reactor in the stirring, 0.5-3h back stopped reaction, supernatant liquor is removed in centrifugation;
8) with in the water-soluble and alcohol mixeding liquid of product, move in the three-necked bottle with storing solution E, feed nitrogen with the airtight back of reactor magnetic stirrer solution, storing solution F is moved in the constant pressure funnel, splash into equably in the reactor in the stirring, 0.5-5h back stopped reaction, centrifugation, remove supernatant liquor,, use absolute ethanol washing three times again with microwave heating 1-8 minute with deionized water wash three times, with twice of deionized water wash, use absolute ethanol washing twice again, product is dissolved in dehydrated alcohol, obtain M
(1-x)Y
2S
4: A
x/ ZnS core/shell structure quantum dot.
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|---|---|---|---|
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103627399A (en) * | 2013-12-13 | 2014-03-12 | 中国科学院长春应用化学研究所 | Semiconductor/fluorescent powder heterostructure and preparation method thereof |
| CN103642495A (en) * | 2013-12-13 | 2014-03-19 | 中国科学院长春应用化学研究所 | Luminescent material with core-shell structure and preparation method thereof |
| CN103694988A (en) * | 2013-11-29 | 2014-04-02 | 南京工业大学 | Preparation method of fluorescent material by utilizing II-VI-group quantum dots instead of rare earth ions |
| CN105713613A (en) * | 2016-01-22 | 2016-06-29 | 华南理工大学 | Rare earth doped quantum dot material for light conversion of solar cells and preparation of rare earth doped quantum dot material |
-
2006
- 2006-12-12 CN CN 200610130073 patent/CN1974720A/en active Pending
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103694988A (en) * | 2013-11-29 | 2014-04-02 | 南京工业大学 | Preparation method of fluorescent material by utilizing II-VI-group quantum dots instead of rare earth ions |
| CN103627399A (en) * | 2013-12-13 | 2014-03-12 | 中国科学院长春应用化学研究所 | Semiconductor/fluorescent powder heterostructure and preparation method thereof |
| CN103642495A (en) * | 2013-12-13 | 2014-03-19 | 中国科学院长春应用化学研究所 | Luminescent material with core-shell structure and preparation method thereof |
| CN103642495B (en) * | 2013-12-13 | 2015-05-20 | 中国科学院长春应用化学研究所 | Luminescent material with core-shell structure and preparation method thereof |
| CN105713613A (en) * | 2016-01-22 | 2016-06-29 | 华南理工大学 | Rare earth doped quantum dot material for light conversion of solar cells and preparation of rare earth doped quantum dot material |
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