CN1868893A - Preparation method of cadmium selenide nano-cluster - Google Patents

Preparation method of cadmium selenide nano-cluster Download PDF

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Publication number
CN1868893A
CN1868893A CN 200610016907 CN200610016907A CN1868893A CN 1868893 A CN1868893 A CN 1868893A CN 200610016907 CN200610016907 CN 200610016907 CN 200610016907 A CN200610016907 A CN 200610016907A CN 1868893 A CN1868893 A CN 1868893A
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cadmium
solution
cluster
cadmium selenide
selenide nano
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CN 200610016907
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Chinese (zh)
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汪尔康
包海峰
黄利坚
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Changchun Institute of Applied Chemistry of CAS
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Changchun Institute of Applied Chemistry of CAS
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Priority to CN 200610016907 priority Critical patent/CN1868893A/en
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Abstract

A process for preparing the cadmium selenide nanolumps able to be used as monoelectron device includes such steps as filling distilled water into a three-opening reactor twice under the protection of Ar gas while stirring, proportionally adding CdCl2 solution and bihydrated trisodium citrate, heating, adding Na2SeSO3 solution, and reacting for 15-120 min.

Description

The preparation method of cadmium selenide nano-cluster
Technical field
The present invention relates to a kind of preparation method of cadmium selenide nano-cluster.
Background technology
The light of semiconductor nano, electrical property can be adjusted by changing its physical size, and can produce the higher emission light of purity of color, and they have demonstrated bright application prospect at aspects such as opto-electronic device and biological fluorescent labellings.Two ten years in the past, the scientists development has also been grasped the nanocrystalline method of synthetic high-quality semiconductor, has prepared nanocrystalline that distribution of sizes becomes very narrow, fluorescence quantum yield is very high.Experimental result points out that nanocrystalline fluorescence quantum yield and nanocrystalline surface properties have much relations.Because nanocrystalline specific surface area is very big, surperficial key attitude and electron energy state are different from granule interior, do not have coordinate to hang key in a large number if particle surface exists, and will cause the formation of some additional defect energy levels in energy gap.In this case, when exciting light acts on semiconductor nano, except the band edge fluorescent emission bands of a spectrum that produce relative narrower, also can produce the defect state photoluminescent band of a broad at the longer wavelength place.This often takes place in synthetic semiconductor nano at a lower temperature.For the nanocrystalline quantum confined effect with good crystalline structure, band theory can provide good explanation.And for unordered semiconductor nano material, band theory just not necessarily has been suitable for, need to explain with " Mott-CFO (model of Mo Te-Ke Fuao) " (referring to: top grade work, " electronic processes in the non-crystalline material (second edition) ", England Oxford Ke Lairuideng press, version (N.F.Mott in 1979, et al, ElectronicProcesses In Non-Crystalline Materials (Second Edition), Clarendon Press, Oxford, 1979)).This model is the most basic model of electron energy state in the non-crystalline state system.When the disordered semiconductor volume-diminished of body phase to nanoscale, and the time less than the spatial dimension of anderson localization, in the disordered semiconductor material of this nano-scale, the expansion attitude disappears, localized state is because quantum confined effect can become isolating energy level, and this moment, the disordered semiconductor material of nanoscale also can show the photoelectric characteristic similar with above-mentioned nanocrystalline material.Therefore, the disordered semiconductor material of these nano-scales can be directly used in the semiconducter device that has and littler nanoparticle needn't be used.Yet, up to the present, also do not have the report of synthetic these nanoclusters.
Summary of the invention
The objective of the invention is to propose a kind of preparation method of cadmium selenide nano-cluster.The present invention adopts the water method to synthesize a kind of cadmium selenide of disordered structure (CdSe) nanoclusters for the first time.
Step of the present invention and condition are: respectively with dichloride cadmium (CdCl 2) and sodium thiosulfate (Na 2SeSO 3) be cadmium source and selenium source.The mol ratio of cadmium and selenium is 10: 1～10; The mol ratio of dichloride cadmium and two hydration trisodium citrates is 2.1: 1.
Under argon shield and stirring, in three mouthfuls of reactors, replenish redistilled water earlier to regulate cumulative volume, making the cadmium concentration in the final blending reaction solution is 3.2moll -1, add CdCl then in proportion respectively 2Solution and two hydration trisodium citrates, and be heated to 80～100 ℃, then in reaction solution, inject Na 2SeSO 3Solution also picks up counting, and stops to heat the cadmium selenide nano-cluster that promptly obtains the protection of 17～25nm Trisodium Citrate behind reaction 15～120min.
Synthetic CdSe nanoclusters is a kind of disordered system nano material of novelty by this method, though this nanoclusters is of a size of about 20nm, the scope that has exceeded Bohr radius, but still show and be similar to the relevant fluorescence phenomenon of the nanocrystalline particle diameter of CdSe, may provide new thinking for studying nano amorphous material, and because the unordered potential well in Anderson can make nanoclusters can realize that the quantum of room temperature discharges and recharges, and becomes the functional element of room temperature single-electron device.
Description of drawings
A among Fig. 1, b, c correspond respectively to the room temperature emmission spectrum and the excitation spectrum of the CdSe nanoclusters that embodiment 1～3 obtains.
A among Fig. 2, B, C correspond respectively to the transmission electron microscope picture (corresponding median size is respectively 17nm, 22nm, 25nm) of the CdSe nanoclusters that embodiment 1～3 obtains
Embodiment
Embodiment 1:
Under argon shield and stirring, in there-necked flask, add the 42ml redistilled water, adding 4ml concentration respectively is 0.04mol.l -1CdCl 2Solution (0.16mmol) and 100mg two hydration trisodium citrates (0.34mmol), injecting 4ml concentration after being heated to 100 ℃ is 0.01mol.l -1Na 2SeSO 3(0.04mmol) solution and picking up counting stops to heat behind the reaction 15min and promptly obtains the CdSe nanoclusters that median size is the Trisodium Citrate protection of 17nm.
Embodiment 2:
Under argon shield and stirring, in there-necked flask, add the 42ml redistilled water, adding 4ml concentration respectively is 0.04mol.l -1CdCl 2Solution (0.16mmol) and 100mg two hydration trisodium citrates (0.34mmol), injecting 4ml concentration after being heated to 100 ℃ is 0.01mol.l -1Na 2SeSO 3(0.04mmol) solution and picking up counting stops to heat behind the reaction 40min and promptly obtains the CdSe nanoclusters that median size is the Trisodium Citrate protection of 22nm.
Embodiment 3:
Under argon shield and stirring, in there-necked flask, add the 42ml redistilled water, adding 4ml concentration respectively is 0.04mol.l -1CdCl 2Solution (0.16mmol) and 100mg two hydration trisodium citrates (0.34mmol), injecting 4ml concentration after being heated to 100 ℃ is 0.01mol.l -1Na 2SeSO 3(0.04mmol) solution and picking up counting stops to heat behind the reaction 120min and promptly obtains the CdSe nanoclusters that median size is the Trisodium Citrate protection of 25nm.
Embodiment 4:
Under argon shield and stirring, in there-necked flask, add the 42ml redistilled water, adding 4ml concentration respectively is 0.04mol.l -1CdCl 2Solution (0.16mmol) and 100mg two hydration trisodium citrates (0.34mmol), injecting 4ml concentration after being heated to 80 ℃ is 0.004mol.l -1Na 2SeSO 3(0.016mmol) solution and picking up counting stops to heat behind the reaction 120min and promptly obtains the CdSe nanoclusters that median size is the Trisodium Citrate protection of 23nm.
Embodiment 5:
Under argon shield and stirring, in there-necked flask, add the 42ml redistilled water, adding 4ml concentration respectively is 0.04mol.l -1CdCl 2Solution (0.16mmol) and 100mg two hydration trisodium citrates (0.34mmol), injecting 4ml concentration after being heated to 90 ℃ is 0.04mol.l -1Na 2SeSO 3(0.16mmol) solution and picking up counting stops to heat behind the reaction 90min and promptly obtains the CdSe nanoclusters that median size is the Trisodium Citrate protection of 22nm.

Claims (1)

1, a kind of preparation method of cadmium selenide nano-cluster is characterized in that, step and condition are: respectively with dichloride cadmium (CdCl 2) and sodium thiosulfate (Na 2Se SO 3) be cadmium source and selenium source, the mol ratio of cadmium and selenium is 10: 1～10, the mol ratio of dichloride cadmium and two hydration trisodium citrates is 2.1: 1; Under argon shield and stirring, in three mouthfuls of reactors, replenish redistilled water earlier to regulate cumulative volume, making the cadmium concentration in the final blending reaction solution is 3.2moll -1, add CdCl then in proportion respectively 2Solution and two hydration trisodium citrates, and be heated to 80～100 ℃, then in reaction solution, inject Na 2SeSO 3Solution also picks up counting, and stops heating behind reaction 15～120min, promptly obtains the cadmium selenide nano-cluster of Trisodium Citrate protection.
CN 200610016907 2006-06-02 2006-06-02 Preparation method of cadmium selenide nano-cluster Pending CN1868893A (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN100557091C (en) * 2007-11-07 2009-11-04 华东理工大学 A kind of micro-reaction device and method of utilizing the thermograde synthesizing cadmium selenide nano-crystal
CN105253861A (en) * 2015-11-03 2016-01-20 中国科学院半导体研究所 Composite nanometer material and preparation method of composite nanometer material

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN100557091C (en) * 2007-11-07 2009-11-04 华东理工大学 A kind of micro-reaction device and method of utilizing the thermograde synthesizing cadmium selenide nano-crystal
CN105253861A (en) * 2015-11-03 2016-01-20 中国科学院半导体研究所 Composite nanometer material and preparation method of composite nanometer material
CN105253861B (en) * 2015-11-03 2017-10-24 中国科学院半导体研究所 A kind of composite nano materials and preparation method thereof

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