CN103145177A - Preparation method of zinc cadmium sulfide nanorod - Google Patents
Preparation method of zinc cadmium sulfide nanorod Download PDFInfo
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- CN103145177A CN103145177A CN2013100023117A CN201310002311A CN103145177A CN 103145177 A CN103145177 A CN 103145177A CN 2013100023117 A CN2013100023117 A CN 2013100023117A CN 201310002311 A CN201310002311 A CN 201310002311A CN 103145177 A CN103145177 A CN 103145177A
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- cadmium sulfide
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Abstract
The invention provides a preparation method of a zinc cadmium sulfide nanorod in the technical field of photoelectric materials. The preparation method comprises the following steps: zinc acetate, cadmium acetylacetonate and powdered sulfur are added into oleylamine/ oleic acid mixture, then mixing, heating, heat-preservation and purification treatment are carried out, and finally the finished product zinc cadmium sulfide nanorod is obtained. The preparation method of the zinc cadmium sulfide nanorod is free of pollution, simple in procedure, easy to operate, simple in reaction condition, simple in process, and suitable for industrialized mass production. An energy band interval of the prepared zinc cadmium sulfide nanorod is capable of varying with the variation of the zinc content, when the zinc content increases from 18% (the molar ratio between zinc and cadmium is 0.18:0.82) to 89% (the molar ratio between the zinc and the cadmium is 0.89:0.11), and the energy band interval increases from 2.62 eV to 3.47 eV and is basically in a linear relationship.
Description
Technical field
The present invention relates to the photoelectric material technical field, particularly, relate to a kind of preparation method of zinc-cadmium sulfide nanometer rod.
Background technology
In recent years, II-VI family semi-conductor is subject to extensive concern owing to having relatively wide band gap and relative simple synthetic method in fields such as solar cell and photochemical catalysis.Wherein, one dimension or quasi-one-dimensional nanometer material are being played the part of important role in nano-device is used, therefore be widely reported about the nano wire of the binary compounds such as zinc oxide (ZnO), zinc selenide (ZnSe), cadmium telluride (CdTe) or the research of nanometer rod.In addition, some ternary compounds, such as zinc-cadmium sulfide (ZnCdS), cadmium-zinc selenide (ZnCdSe) etc., the adjusting by composition has possessed continuously adjustable band gap, more is conducive to the application in association area in the future of such material.
Through the literature search of prior art is found, S.Sain etc. are at " Journal of Alloys and Compounds " (alloy and compound magazine) the 509th the 10th phase of volume 4176-4184 page in 2011 " Mechanochemical solid state synthesis of (Cd that publishes an article
0.8Zn
0.2) S quantum dots:Microstructure and optical characterizations " (the solid-state synthetic zinc-cadmium sulfide quantum dot of mechanochemical reaction and microtexture and optical property research); and then the zinc-cadmium sulfide of the different morphologies such as nano wire or nanometer rod is synthesized successively.
Summary of the invention
For defective of the prior art, the purpose of this invention is to provide a kind of preparation method of zinc-cadmium sulfide nanometer rod.
The present invention realizes by following technological method,
The present invention relates to a kind of preparation method of zinc-cadmium sulfide nanometer rod, comprise the steps:
With zinc acetate, the methyl ethyl diketone cadmium, the sulphur powder adds in oleyl amine/oleic acid mixture, mixes, heating, insulation, purification process namely gets final product zinc-cadmium sulfide nanometer rod.
Preferably, the mol ratio of the oleyl amine in described oleyl amine/oleic acid mixture and oleic acid is 9: 1.
Preferably, described zinc acetate, the methyl ethyl diketone cadmium, the sulphur powder adds the mol ratio of oleyl amine/oleic acid mixture to be (0.4～1.8): (0.2～1.6): 8: (2～8).
Preferably, described Heating temperature is 260～300 ℃, and described soaking time is 1～2 hour.
Preferably, the diameter of described zinc-cadmium sulfide nanometer rod is 6～8nm.
Compared with prior art, the present invention has following beneficial effect:
(1) the zinc-cadmium sulfide nanometer rod of the inventive method preparation, its band gap can change with the zinc content; When zinc content rose to 89% (zinc: the cadmium mol ratio is 0.89: 0.11) from 18% (zinc: the cadmium mol ratio is 0.18: 0.82), band gap rose to 3.47eV from 2.62eV, and substantially presents linear relationship;
(2) the inventive method is pollution-free, and step is simple, easily operation, and reaction conditions is simple, and technique is simple, and is pollution-free, is fit to large-scale industrialization production.
Description of drawings
By reading the detailed description of non-limiting example being done with reference to the following drawings, it is more obvious that other features, objects and advantages of the present invention will become:
Fig. 1 is the transmission electron microscope photo of the zinc-cadmium sulfide nanometer rod of the embodiment of the present invention 1 preparation;
Fig. 2 is the transmission electron microscope photo of the zinc-cadmium sulfide nanometer rod of the embodiment of the present invention 2 preparations;
Fig. 3 is the transmission electron microscope photo of the zinc-cadmium sulfide nanometer rod of the embodiment of the present invention 3 preparations.
Embodiment
The present invention is described in detail below in conjunction with specific embodiment.Following examples will help those skilled in the art further to understand the present invention, but not limit in any form the present invention.Should be pointed out that to those skilled in the art, without departing from the inventive concept of the premise, can also make some distortion and improvement.These all belong to protection scope of the present invention.
Embodiment 1
The present embodiment provides a kind of preparation method of zinc-cadmium sulfide nanometer rod, comprises the steps:
Get 1.8mmol zinc acetate, 0.2mmol methyl ethyl diketone cadmium, 8mmol sulphur powder; Add afterwards reaction tubes, then add in 2mmol oleyl amine/oleic acid mixture (mol ratio of oleyl amine and oleic acid is 9: 1), solution is placed under the atmosphere of nitrogen, be warming up to 300 ℃ and be incubated 1 hour; Afterwards, products therefrom is carried out purifying, be specially: product is dissolved in ethanol, after ultrasonic separation and with 12000rpm centrifugal 10 minutes; Take off layer precipitation, add ultrasonic separation after chloroform, then add ultrasonic separation after ethanol, then with 12000rpm centrifugal 10 minutes, take off layer precipitation; Add ultrasonic separation after chloroform, then add the ethanol ultrasonic separation, take off at last layer precipitation with 12000rpm after centrifugal 10 minutes, solvent evaporated obtains the zinc-cadmium sulfide nanometer rod.
Implementation result, as shown in Figure 1, the zinc-cadmium sulfide nanometer rod diameter of the present embodiment preparation is 8nm, records by EDS that in product, zinc content is 89% (zinc: the cadmium mol ratio is 0.89: 0.11).
Embodiment 2
The present embodiment provides a kind of preparation method of zinc-cadmium sulfide nanometer rod, comprises the steps:
Get 1mmol zinc acetate, 1mmol methyl ethyl diketone cadmium, 8mmol sulphur powder; Add afterwards reaction tubes, then add in 8mmol oleyl amine/oleic acid mixture (mol ratio of oleyl amine and oleic acid is 9: 1), solution is placed under the atmosphere of nitrogen, be warming up to 260 ℃ and be incubated 2 hours; Afterwards, products therefrom is carried out purifying, be specially: product is dissolved in ethanol, after ultrasonic separation and with 12000rpm centrifugal 10 minutes; Take off layer precipitation, add ultrasonic separation after chloroform, then add ultrasonic separation after ethanol, then with 12000rpm centrifugal 10 minutes, take off layer precipitation; Add ultrasonic separation after chloroform, then add the ethanol ultrasonic separation, take off at last layer precipitation with 12000rpm after centrifugal 10 minutes, solvent evaporated obtains the zinc-cadmium sulfide nanometer rod.
Implementation result, as shown in Figure 2, the zinc-cadmium sulfide nanometer rod diameter of the present embodiment preparation is 6nm, records by EDS that in product, zinc content is 51% (zinc: the cadmium mol ratio is 0.51: 0.49).
Embodiment 3
The present embodiment provides a kind of preparation method of zinc-cadmium sulfide nanometer rod, comprises the steps:
Get 0.4mmol zinc acetate, 1.6mmol methyl ethyl diketone cadmium, 8mmol sulphur powder; Add afterwards reaction tubes, then add in 6mmol oleyl amine/oleic acid mixture (mol ratio of oleyl amine and oleic acid is 9: 1), solution is placed under the atmosphere of nitrogen, be warming up to 280 ℃ and be incubated 1.5 hours; Afterwards, products therefrom is carried out purifying, be specially: product is dissolved in ethanol, after ultrasonic separation and with 12000rpm centrifugal 10 minutes; Take off layer precipitation, add ultrasonic separation after chloroform, then add ultrasonic separation after ethanol, then with 12000rpm centrifugal 10 minutes, take off layer precipitation; Add ultrasonic separation after chloroform, then add the ethanol ultrasonic separation, take off at last layer precipitation with 12000rpm after centrifugal 10 minutes, solvent evaporated obtains the zinc-cadmium sulfide nanometer rod.
Implementation result, as shown in Figure 3, the zinc-cadmium sulfide nanometer rod diameter of the present embodiment preparation is 7nm, records by EDS that in product, zinc content is 18% (zinc: the cadmium mol ratio is 0.18: 0.82).
Simultaneously, through the zinc-cadmium sulfide nanometer rod of embodiment 1～3 preparation is verified, when finding that zinc content rises to 89% from 18%, band gap rises to 3.47eV from 2.62eV, and substantially presents linear relationship.
In sum, method of the present invention is synthesized the adjustable zinc-cadmium sulfide nanometer rod of band gap, and the method green non-pollution is simple to the requirement of equipment, is fit to large-scale industrialization production.
Above specific embodiments of the invention are described.It will be appreciated that, the present invention is not limited to above-mentioned specific implementations, and those skilled in the art can make various distortion or modification within the scope of the claims, and this does not affect flesh and blood of the present invention.
Claims (5)
1. the preparation method of a zinc-cadmium sulfide nanometer rod, is characterized in that, comprises the steps:
With zinc acetate, the methyl ethyl diketone cadmium, the sulphur powder adds in oleyl amine/oleic acid mixture, mixes, heating, insulation, purification process namely gets final product zinc-cadmium sulfide nanometer rod.
2. the preparation method of zinc-cadmium sulfide nanometer rod as claimed in claim 1, is characterized in that, in described oleyl amine/oleic acid mixture, the mol ratio of oleyl amine and oleic acid is 9: 1.
3. the preparation method of zinc-cadmium sulfide nanometer rod as claimed in claim 1, is characterized in that, described zinc acetate, and the methyl ethyl diketone cadmium, the sulphur powder, the mol ratio of oleyl amine/oleic acid mixture is (0.4～1.8): (0.2～1.6): 8: (2～8).
4. the preparation method of zinc-cadmium sulfide nanometer rod as claimed in claim 1, is characterized in that, described Heating temperature is 260～300 ℃, and described soaking time is 1～2 hour.
5. the preparation method of zinc-cadmium sulfide nanometer rod as claimed in claim 1, is characterized in that, the diameter of described zinc-cadmium sulfide nanometer rod is 6～8nm.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103588178A (en) * | 2013-11-27 | 2014-02-19 | 闽南师范大学 | Technology for synthesizing sulfur quantum dots through oil-water interface method |
| CN108906125A (en) * | 2018-06-12 | 2018-11-30 | 常州大学 | Three dish alkene polymer DTP/ zinc-cadmium sulfide Cd of one kind0.5Zn0.5The preparation method of S composite photo-catalyst |
| CN109351360A (en) * | 2018-11-13 | 2019-02-19 | 福州大学 | A kind of tantalum polyacid base tri compound light urges agent and its preparation method and application |
| CN110102316A (en) * | 2019-05-07 | 2019-08-09 | 东莞理工学院 | A kind of preparation method of the spherical zinc-cadmium sulfide solid solution of porous nano |
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| CN101130693A (en) * | 2007-09-27 | 2008-02-27 | 上海交通大学 | Method of producing three fundamental quantum dot CdZnSe |
| CN101590413A (en) * | 2009-06-26 | 2009-12-02 | 天津工业大学 | Has visible light-responded Zinc-cadmium sulfide photocatalyst and preparation method thereof |
| US20110033368A1 (en) * | 2007-10-05 | 2011-02-10 | Agency For Science, Technology And Research | Methods of forming a nanocrystal |
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2013
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| CN101130693A (en) * | 2007-09-27 | 2008-02-27 | 上海交通大学 | Method of producing three fundamental quantum dot CdZnSe |
| US20110033368A1 (en) * | 2007-10-05 | 2011-02-10 | Agency For Science, Technology And Research | Methods of forming a nanocrystal |
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| QIULIN NIE ET AL .: "In situ synthesis of ZnxCd1−xS nanorod by a hydrothermal route", 《JOURNAL OF MATERIALS SCIENCE》 * |
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| XINHUA ZHONG ET AL.: "Alloyed ZnxCd1-xS Nanocrystals with Highly Narrow Luminescence Spectral Width", 《J. AM. CHEM. SOC.》 * |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103588178A (en) * | 2013-11-27 | 2014-02-19 | 闽南师范大学 | Technology for synthesizing sulfur quantum dots through oil-water interface method |
| CN108906125A (en) * | 2018-06-12 | 2018-11-30 | 常州大学 | Three dish alkene polymer DTP/ zinc-cadmium sulfide Cd of one kind0.5Zn0.5The preparation method of S composite photo-catalyst |
| CN108906125B (en) * | 2018-06-12 | 2019-11-12 | 常州大学 | Three dish alkene polymer DTP/ zinc-cadmium sulfide Cd of one kind0.5Zn0.5The preparation method of S composite photo-catalyst |
| CN109351360A (en) * | 2018-11-13 | 2019-02-19 | 福州大学 | A kind of tantalum polyacid base tri compound light urges agent and its preparation method and application |
| CN109351360B (en) * | 2018-11-13 | 2020-11-27 | 福州大学 | Tantalum polyacid-based ternary composite photocatalyst and preparation method and application thereof |
| CN110102316A (en) * | 2019-05-07 | 2019-08-09 | 东莞理工学院 | A kind of preparation method of the spherical zinc-cadmium sulfide solid solution of porous nano |
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