CN101311383A - Semiconductor nanocrystalline and method for preparing same - Google Patents
Semiconductor nanocrystalline and method for preparing same Download PDFInfo
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- CN101311383A CN101311383A CNA2008100493380A CN200810049338A CN101311383A CN 101311383 A CN101311383 A CN 101311383A CN A2008100493380 A CNA2008100493380 A CN A2008100493380A CN 200810049338 A CN200810049338 A CN 200810049338A CN 101311383 A CN101311383 A CN 101311383A
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Abstract
The invention relates to a semiconductor nano-crystal and a preparation method thereof. The composition of the semiconductor nano-crystal is as follows: AXB1-XC with x bigger than 0 and smaller than 1; wherein A is Cd or Zn: when A is Cd, B is Hg and C is Te; when A is Zn, B is Cd or Cu and C is Se. During preparation, the CdTe or ZnSe nano-crystal is firstly dissolved in reaction solvent with mercaptan of C4 to C12 as a stabilizer, and then reacts with the solution acquired by dissolving mercury salt, cadmium salt or copper salt in organic solvent while the temperature remains 20 to 100 DEG C, and the semiconductor nano-crystal AXB1-XC is got. The semiconductor nano-crystal prepared by the method has a controllable size, shape and appearance, a high luminous efficiency, and a luminous range which can be adjusted as required. The preparation method has the advantages of simplicity, controllable condition, placid reaction condition and low cost and the preparation method is worth promoting.
Description
(1) technical field
The present invention relates to a kind of semiconductor nano and preparation method thereof, belong to technical field of nano material.
(2) background technology
In recent years, has far infrared and near-infrared luminous nanocrystalline application in biological detection has caused numerous workers' research interest, these are nanocrystalline can effectively to weaken the influence of autofluorescence to detection signal, and its excitation wavelength and emission wavelength be not organized liquid (as water and hemochrome) absorption.What therefore, have an infrared acquisition ability nanocrystallinely has a good application prospects in biological detection.
Near-infrared luminous nanocrystalline round how to use as the application of mapping unit at biological field, currently mainly contain two difficult problems.The first, the synthetic technology of near-infrared nanocrystalline is not well set up; Secondly, the toxicity of near-infrared nanocrystalline and unstable limit its application.At present primary problem be solve how to prepare have super stable, super wide fluorescence emission spectrum, thereby can be widely used in the image intensifer in the wireless radio transmission and the stable near-infrared luminous nanocrystalline problem of biological reflection.
At present, nanocrystalline synthetic technology such as CdSe, CdTe is comparative maturity, the size pattern has also obtained better controlled, but still there are a lot of problems in nanocrystalline the synthesizing of some material, for example the mercury compounds is generally extremely unstable in greater than the organic phases of 100 degree in temperature, be difficult to find controlled synthesis condition, simultaneously also be difficult to obtain for pattern and controllable size, luminous efficiency height, semiconductor nano that light emitting region is adjustable.
(3) summary of the invention
The object of the present invention is to provide a kind of pattern and controllable size, luminous efficiency height, semiconductor nano that light emitting region is adjustable, a kind of this type of preparation of nano crystal also is provided simultaneously, simple to operately be convenient to control, reduced preparation cost.
The technical solution used in the present invention is as follows:
A kind of semiconductor nano, composed as follows: A
XB
1-XC, 0＜x＜1, wherein A is Cd or Zn, and when A was Cd, B was Hg, and C is Te; When A was Zn, B was Cd or Cu, and C is Se.
Described semiconductor nano size range is 2nm-8nm, and luminous efficiency can reach more than 20%; Light emitting region is adjustable, as Cd
xHg
1-xThe nanocrystalline fluorescence radiation scope of Te is 650nm-900nm, Zn
xCd
1-xThe light emitting region of Se is 480-520nm, Zn
xCu
1-xThe light emitting region of Se is 440nm-650nm.
Described semiconductor nano can prepare by the following method:
With CdTe or ZnSe is nanocrystalline is dissolved in the reaction solvent, be stablizer with the mercaptan of C4-C12, the solution that is dissolved in organic solvent with mercury salt, cadmium salt or mantoquita fully acts on then, and keeping temperature is 20-100 ℃, promptly gets described A
XB
1-XThe C semiconductor nano.Mercury, cadmium or the copper that adds is 0.1-2 with the amount of substance of CdTe or ZnSe ratio: 1, and the volume that stablizer adds is 5-10 a times of nanocrystalline amount of substance; The strength of solution that mercury salt, cadmium salt or mantoquita are dissolved in organic solvent be nanocrystalline in reaction solvent concentration 20-100 doubly; Described organic solvent is methyl alcohol, ethanol or Virahol, and described reaction solvent is benzene, toluene, ethylbenzene, dimethylbenzene, normal hexane or chloroform.
The nanocrystalline synthetic method of described raw material CdTe or ZnSe is comparatively ripe, and what ordinary method made gets final product.Present method is to prepare with simple ion exchange method to be difficult to the synthetic semiconductor nano under the usual terms, makes in the past and need also unmanageable reaction at room temperature can carry out under exacting terms such as high temperature, and is very simple, and cost is very low.
Wherein, described mercury salt can be selected mercuric perchlorate, Mercury pernitrate, mercuric acetate or Mercury bisulfate; Described cadmium salt can be cadmium nitrate, cadmium acetate, Cadmium Sulphate, Cadmium chloride fine powder or cadmium phosphate; Described mantoquita can be cupric nitrate, cupric chloride or copper sulfate.The preferred lauryl mercaptan of described stablizer.
When being raw material reaction, should note needing under protection of inert gas, to carry out so that ZnSe is nanocrystalline.
Nanocrystalline and the presoma that present method makes is compared, and pattern and size do not have considerable change, and absorption and fluorescence peak position all are moved, and its fluorescence intensity does not have considerable change, and luminous efficiency is higher.By nanocrystalline luminous of size morphology control, also can make nanocrystalline fluorescence cover the Visible-to-Near InfaRed zone or near infrared region, to reach the purpose that is applied to biological detection and image intensifer simultaneously by controlling two kinds of ionic ratios.Mainly be to be used for branch-like and the brilliant preparation of granular nanometer on nanocrystalline morphology control.
The present invention has following advantage with respect to prior art:
Semiconductor nano size, pattern that the present invention makes are controlled, the luminous efficiency height, and light emitting region can be regulated as required.The preparation method is simple, and condition is controlled controlled easily, and reaction conditions is gentle, and cost is low, is worthy to be popularized.
(4) description of drawings
Fig. 1 is the nanocrystalline Electronic Speculum transmission photo of CdTe;
The Electronic Speculum transmission photo of the semiconductor nano that Fig. 2 makes for embodiment 1;
The Electronic Speculum transmission photo of the semiconductor nano that Fig. 3 makes for embodiment 2;
The Electronic Speculum transmission photo of the semiconductor nano that Fig. 4 makes for embodiment 3;
The Electronic Speculum transmission photo of the semiconductor nano that Fig. 5 makes for embodiment 4;
The ultraviolet-visible absorption spectroscopy of the semiconductor nano that Fig. 6 makes for embodiment 1-4;
The fluorescence spectrum of the semiconductor nano that Fig. 7 makes for embodiment 1-4;
The fluorescence spectrum of the semiconductor nano that Fig. 8 makes for embodiment 5.
(5) embodiment:
Below with specific embodiment technical scheme of the present invention is described, but protection scope of the present invention is not limited thereto:
Embodiment 1
Compound concentration is 1.3 * 10
-2The CdTe toluene solution of mol/L is got this solution of 2.1ml, adds the 0.2ml lauryl mercaptan under the room temperature while stirring, and then adds the Hg (ClO of 0.02ml 0.335mol/L
4) 3H
2The O methanol solution stirred 10 minutes, became brownly from scarlet up to solution, obtained the dendritic Hg of branch
0.2Cd
0.8Te is nanocrystalline.The nanocrystalline Electronic Speculum transmission photo of CdTe is seen Fig. 1, the Hg that makes
0.2Cd
0.8The nanocrystalline Electronic Speculum transmission of Te photo is seen Fig. 2, and ultraviolet-visible absorption spectroscopy is seen Fig. 6, and fluorescent absorption spectrum is seen Fig. 7.
Embodiment 2-4
Add Hg (ClO
4) 3H
2The amount of O methanol solution is respectively 0.027ml, 0.04ml and 0.06ml, and other obtain the dendritic semiconductor nano Hg of branch respectively with embodiment 1 after stirring
0.25Cd
0.75Te, Hg
0.33Cd
0.67Te and Hg
0.43Cd
0.57Te, transmission electron microscope photo see Fig. 3, Fig. 4, Fig. 5 respectively, and ultraviolet-visible absorption spectroscopy is seen Fig. 6, and fluorescent absorption spectrum is seen Fig. 7.
Embodiment 5
Compound concentration is 5.2 * 10
-3The ZnSe toluene solution 4ml of mol/L; logical nitrogen protection; stir and add the 0.018ml lauryl mercaptan down; be heated to 60 ℃; divide three each 0.3ml to inject the cadmium nitrate solution that 0.9mL concentration is 0.1M altogether; when 6min; be warming up to 100 degree and keep this temperature always; 8 minutes and 18 minutes difference sampling and measurings; fluorescent spectrum curve is seen a and the b of Fig. 8 respectively; the 0.3mL cadmium nitrate solution that reinjects in the time of 45 minutes continues reaction 18 minutes and 30 minutes sampling and measuring, and its fluorescence spectrum figure sees curve c and the d of Fig. 8 respectively.Be to add excessive reactant, the spectrum of the semiconductor nano that measures over time in this example.
Claims (6)
1. a semiconductor nano is characterized in that described semiconductor nano is composed as follows: A
XB
1-XC, 0＜x＜1, wherein A is Cd or Zn:A when being Cd, and B is Hg, and C is Te; When A was Zn, B was Cd or Cu, and C is Se.
2. the preparation method of semiconductor nano as claimed in claim 1, it is characterized in that earlier CdTe or ZnSe is nanocrystalline is dissolved in the reaction solvent, mercaptan with C4-C12 is stablizer, the solution that is dissolved in organic solvent with mercury salt, cadmium salt or mantoquita fully acts on then, keeping temperature is 20-100 ℃, promptly gets A
XB
1-XThe C semiconductor nano, 0＜x＜1, wherein A is Cd or Zn:A when being Cd, and B is Hg, and C is Te; When A was Zn, B was Cd or Cu, and C is Se; Mercury, cadmium or the copper that adds is 0.1-2 with the amount of substance of CdTe or ZnSe ratio: 1, and the volume that stablizer adds is 5-10 a times of nanocrystalline amount of substance; The strength of solution that mercury salt, cadmium salt or mantoquita are dissolved in organic solvent be nanocrystalline in reaction solvent concentration 20-100 doubly; Described organic solvent is methyl alcohol, ethanol or Virahol, and described reaction solvent is benzene, toluene, ethylbenzene, dimethylbenzene, normal hexane or chloroform.
3. the preparation method of semiconductor nano as claimed in claim 2 is characterized in that described mercury salt is mercuric perchlorate, Mercury pernitrate, mercuric acetate or Mercury bisulfate.
4. the preparation method of semiconductor nano as claimed in claim 2 is characterized in that described cadmium salt is cadmium nitrate, cadmium acetate, Cadmium Sulphate, Cadmium chloride fine powder or cadmium phosphate.
5. the preparation method of semiconductor nano as claimed in claim 2 is characterized in that described mantoquita is cupric nitrate, cupric chloride or copper sulfate.
6. the preparation method of semiconductor nano as claimed in claim 2 is characterized in that described stablizer is a lauryl mercaptan.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101554999B (en) * | 2009-04-30 | 2012-02-22 | 河南大学 | Method for synthesizing tellurium-contained semiconductor nanocrystal |
| CN103059872A (en) * | 2013-01-28 | 2013-04-24 | 武汉大学 | Method for synthesizing Zn doped with CdTe quantum dots in one step |
| KR20190124868A (en) * | 2018-04-27 | 2019-11-06 | 고려대학교 산학협력단 | Quantum dot capable of controlling electronic transition in smaller region than inherent bandgap beyond inherent absorption and emission region of quantum dot material, and furthermore controlling electronic transition into localized surface plasmon resonance region |
| CN110983425A (en) * | 2019-12-31 | 2020-04-10 | 中国科学技术大学 | Ag2HgS2Single crystal and method for producing the same |
| CN111977617A (en) * | 2019-05-22 | 2020-11-24 | 北京理工大学 | Method for preparing cadmium-based alloy nano material |
| CN115477947A (en) * | 2022-08-19 | 2022-12-16 | 华中科技大学 | Mercury-based chalcogenide quantum dot, preparation method thereof and sensor |
Family Cites Families (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100509635C (en) * | 2007-01-15 | 2009-07-08 | 山东师范大学 | Method for synthesizing water-soluble Nano CdllgTe stick, and usage of Nano stick |
| CN100529013C (en) * | 2007-09-27 | 2009-08-19 | 上海交通大学 | Method of producing three fundamental quantum dot CdZnSe |
-
2008
- 2008-03-11 CN CN2008100493380A patent/CN101311383B/en active Active
Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101554999B (en) * | 2009-04-30 | 2012-02-22 | 河南大学 | Method for synthesizing tellurium-contained semiconductor nanocrystal |
| CN103059872A (en) * | 2013-01-28 | 2013-04-24 | 武汉大学 | Method for synthesizing Zn doped with CdTe quantum dots in one step |
| CN103059872B (en) * | 2013-01-28 | 2014-03-26 | 武汉大学 | Method for synthesizing Zn doped with CdTe quantum dots in one step |
| KR20190124868A (en) * | 2018-04-27 | 2019-11-06 | 고려대학교 산학협력단 | Quantum dot capable of controlling electronic transition in smaller region than inherent bandgap beyond inherent absorption and emission region of quantum dot material, and furthermore controlling electronic transition into localized surface plasmon resonance region |
| KR102084675B1 (en) | 2018-04-27 | 2020-03-04 | 고려대학교 산학협력단 | Controlling method of the intraband electronic transition in the quantum dot |
| CN111977617A (en) * | 2019-05-22 | 2020-11-24 | 北京理工大学 | Method for preparing cadmium-based alloy nano material |
| CN111977617B (en) * | 2019-05-22 | 2022-05-17 | 北京理工大学 | Method for preparing cadmium-based alloy nano material |
| CN110983425A (en) * | 2019-12-31 | 2020-04-10 | 中国科学技术大学 | Ag2HgS2Single crystal and method for producing the same |
| CN115477947A (en) * | 2022-08-19 | 2022-12-16 | 华中科技大学 | Mercury-based chalcogenide quantum dot, preparation method thereof and sensor |
| CN115477947B (en) * | 2022-08-19 | 2023-12-19 | 华中科技大学 | Mercury-based chalcogen compound quantum dot, preparation method thereof and sensor |
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|---|---|
| CN101311383B (en) | 2012-04-18 |
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