CN101214932A - Method for preparing nanometer tin selenide - Google Patents
Method for preparing nanometer tin selenide Download PDFInfo
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- CN101214932A CN101214932A CNA2008100324185A CN200810032418A CN101214932A CN 101214932 A CN101214932 A CN 101214932A CN A2008100324185 A CNA2008100324185 A CN A2008100324185A CN 200810032418 A CN200810032418 A CN 200810032418A CN 101214932 A CN101214932 A CN 101214932A
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- tin selenide
- ethylenediamine
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Abstract
The invention relates to a method of preparing nano tin selenide, and belongs to the technical field of nano material processes. In the method of the invention, selenium powder dissolves into the ethylenediamine solution in ethylenediamine which can prepare selenium, SnCl22H2O is dissolved into distilled water to prepare solution of Sn2+; the ethylenediamine solution of selenium is slowly poured into the solution of Sn2+ to be continuously mixed; after isopropanol is added in, the solution is poured into a sealed container to receive irradiation treatment by electron beam; and then the product is repeatedly washed, cleaned and separated; the precipitate is dried, and the black nano tin selenide powder is obtained. The method of the invention is characterized by simple manufacturing process, short cycle, high yield, good safety, no pollution, operation under room temperature, no need of any catalyst and chemical initiator, etc. The nano tin selenide obtained through the method of the invention has high purity, superior optical performance, and thus has broad application prospect.
Description
Technical field:
The present invention relates to a kind of preparation method of nanometer tin selenide, belong to radiation chemistry and make nano material Technology field.
Background technology:
The crystalline state nanometer semiconductor particle has caused the extensive concern of scientific circles because of it has big surface volume than, high activity, special electrical properties and unique optical property.The quantum size effect of based semiconductor nanoparticle and surface effects.Semi-conductor nano particles has broad application prospects at aspects such as luminescent material, nonlinear optical material, photosensor material, photocatalyst materials.Tin diselenide (SnSe) has boundless application prospect as IV-VI family semiconductor compound.SnSe is a kind of important semiconductor material, energy gap is about 0.9eV, anisotropy, similar is in spacer, have excellent electricity, optical property, be widely used in the solid-phase media of infrared electro instrument and memory change-over switch, thermoelectric-cooled material, spectral filter, optical writing material, solar cell material, super ionic material, transmitter and laserable material, hologram etc.; Sheet SnSe also can be used as the cathode material of lithium ion battery.
The at present existing multiple method for preparing nanometer tin selenide comprises Bridgman method, solid state reaction, hydrothermal method, solvent-thermal method, organometallic precursor method, electrochemical deposition method etc.These methods have complex process usually, need high temperature, long reaction time.And shortcoming such as most of organometallic precursor are poisonous.The inventive method adopts radiation method to prepare nanometer tin selenide, and this invented technology flow process is simple, with short production cycle, and is pollution-free and security good.
Summary of the invention:
The object of the present invention is to provide a kind of preparation method of nanometer tin selenide.
For achieving the above object, the present invention adopts following technical scheme:
A kind of preparation method of nanometer tin selenide is characterized in that this method has following processing step:
A. at first, take by weighing a certain amount of selenium powder with electronic balance, it is dissolved in the quadrol and fully stirs, the preparation selenium concentration is the selenium ethylenediamine solution of 0.005-0.01mol/100ml; Take by weighing a certain amount of SnCl with electronic balance then
22H
2O is dissolved in the distilled water, and compound concentration is 0.005-0.01mol/100ml Sn
2+Solution.Slowly pour the ethylenediamine solution of selenium into Sn
2+Solution in, constantly stir it fully disperseed, obtain as clear as crystal mixing solutions, add Virahol as the oxidative free radical scavenging agent, add-on is 3-5ml/100ml, in the container of then solution being packed into and sealing;
B. the above-mentioned sealed vessel that fills the solution for preparing is placed on 2MeV, carries out radiation treatment under the irradiation of the electron beam that ground that meter rumbatron of 10mA produces, its irradiation dose is 300-400KGy;
C. use the sample of absolute ethanol washing then, clean with distilled water again through irradiation, and centrifugation in supercentrifuge, repeatedly for several times, to remove unreacted ion and quadrol in the solution;
D. throw out is dry in baking oven, temperature is 60 ℃, and drying time is 3-5 hour, finally can obtain the nanometer tin selenide powder of black.
The present invention proposes the electron beam irradiation legal system and be equipped with nanometer tin selenide, with selenium powder and SnCl
22H
2O is a raw material, and quadrol is a tensio-active agent, and the electron beam that uses electron-beam accelerator to produce carries out radiation treatment, and the solution behind the irradiation is cleaned, separates, dries, and can obtain highly purified nanometer tin selenide.Pollution-free in this method radiation synthesis process, can prepare the uniform Tin diselenide particle of nanoscale fast, technology is simple simultaneously, does not have any intermediate product, and is easy to operate, can realize suitability for industrialized production.
Compare with prior art, the inventive method is owing to the preparation that the electron beam irradiation technology is applied to nanometer tin selenide, thereby it is simple to have preparation technology, can operate at normal temperatures, does not add any catalyzer and chemical initiator, and preparation cycle is short; Product controllable granularity and productive rate height, security are good, characteristics such as pollution-free.The nanometer tin selenide purity height that adopts the inventive method to obtain, superb optical performance, powder particle is tiny evenly, and shape is complete.Thereby this method has extremely wide research and application prospect.
Description of drawings
The XRD figure of the nanometer SnSe of Fig. 1 electron beam irradiation method preparation
Embodiment
Now in conjunction with the embodiments the present invention further is described in the back:
The concrete preparation process of present embodiment is as follows:
A. take by weighing a certain amount of selenium powder with electronic balance, it is dissolved in the quadrol fully stirs, wherein selenium concentration reaches 0.005mol/100ml; Electronic balance takes by weighing a certain amount of SnCl then
22H
2O is dissolved in the distilled water, and compound concentration is 0.005mol/100ml Sn
2+Solution.Slowly pour the ethylenediamine solution of selenium into Sn
2+Solution in, constantly stir it fully disperseed, obtain as clear as crystal mixing solutions, add Virahol as the oxidative free radical scavenging agent, add-on is 3ml/100ml, seals in the container of then solution being packed into;
B. the above-mentioned sealed vessel that fills the solution for preparing is placed on 2MeV, carries out radiation treatment under the irradiation of the electron beam that ground that meter rumbatron of 10mA produces, its irradiation dose is 350KGy;
C. use the sample of absolute ethanol washing then, clean with distilled water again through irradiation, and centrifugation in supercentrifuge, repeated multiple times is to remove unreacted ion and quadrol in the solution;
D. throw out is dry in baking oven, temperature is 60 ℃, and drying time is 5 hours, finally obtains the nanometer tin selenide powder of black.
Utilize X-ray diffraction analysis method (the results are shown in Figure 1), transmission electron microscope and ultraviolet-visible light spectrum analysis are analyzed sample.Gained is the result prove, the sample for preparing in the present embodiment is a nanometer tin selenide, does not contain any impurity, and average nanoparticle size is 10nm.Sample is that 580nm (energy gap is 1.8eV) has located the last one glow peak at wavelength, and tangible blue shift has all taken place the energy gap with respect to SnSe agglomerate crystal 0.9eV.Utilize this optical characteristics, nanometer tin selenide will have broad application prospects at aspects such as battery material, super ionic material, transmitter and laserable materials.
Claims (1)
1. the preparation method of a nanometer tin selenide is characterized in that this method has following processing step:
A. at first, take by weighing a certain amount of selenium powder with electronic balance, it is dissolved in the quadrol and fully stirs, the preparation selenium concentration is the selenium ethylenediamine solution of 0.005-0.01mol/100ml; Take by weighing a certain amount of SnCl with electronic balance then
22H
2O is dissolved in the distilled water, and compound concentration is 0.005-0.01mol/100ml Sn
2+Solution.Slowly pour the ethylenediamine solution of selenium into Sn
2+Solution in, constantly stir it fully disperseed, obtain as clear as crystal mixing solutions, add Virahol as the oxidative free radical scavenging agent, add-on is 3-5ml/100ml, in the container of then solution being packed into and sealing;
B. the above-mentioned sealed vessel that fills the solution for preparing is placed on 2MeV, carries out radiation treatment under the irradiation of the electron beam that ground that meter rumbatron of 10mA produces, its irradiation dose is 300-400KGy;
C. use the sample of absolute ethanol washing then, clean with distilled water again through irradiation, and centrifugation in supercentrifuge, repeatedly for several times, to remove unreacted ion and quadrol in the solution;
D. throw out is dry in baking oven, temperature is 60 ℃, and drying time is 3-5 hour, finally can obtain the nanometer tin selenide powder of black.
Priority Applications (1)
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| CNA2008100324185A CN101214932A (en) | 2008-01-08 | 2008-01-08 | Method for preparing nanometer tin selenide |
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Cited By (14)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101412505B (en) * | 2008-09-05 | 2010-06-02 | 山东建筑大学 | Preparation of high-purity tin diselenide nano-plate |
| CN101920942A (en) * | 2010-09-20 | 2010-12-22 | 东华大学 | Method for controlling synthesis of zinc selenide multi-morphological nano material |
| CN101585518B (en) * | 2009-06-26 | 2011-03-30 | 上海大学 | Method for fast synthesizing powder of stannum selenide quanta dots |
| CN102897724A (en) * | 2012-09-06 | 2013-01-30 | 江苏大学 | Tin selenide nano-flowers and preparation method thereof |
| CN104692342A (en) * | 2015-02-17 | 2015-06-10 | 吉林大学 | Preparation method of stannous selenide nanospheres |
| CN104692343A (en) * | 2015-03-17 | 2015-06-10 | 福州大学 | Tin selenide nano material, preparation method and application thereof |
| CN104692341A (en) * | 2015-02-17 | 2015-06-10 | 吉林大学 | SnSe square nanosheets and preparation method thereof |
| CN104831362A (en) * | 2015-06-08 | 2015-08-12 | 广东工业大学 | Method for preparing tin selenide single-crystal nano-belt |
| CN105032451A (en) * | 2015-08-03 | 2015-11-11 | 广东工业大学 | Application of tin selenide nanometer material in photocatalysis aspect |
| CN106744727A (en) * | 2016-11-28 | 2017-05-31 | 福建师范大学 | Screw dislocation drives the preparation method of growth spiral type stratiform stannic selenide nanometer sheet |
| CN107381514A (en) * | 2017-08-09 | 2017-11-24 | 同济大学 | A kind of method of microwave radiation technology Fast back-projection algorithm stannic selenide nanometer sheet |
| CN109811428A (en) * | 2019-01-31 | 2019-05-28 | 湘潭大学 | A kind of electrostatic spinning preparation method of flexibility SnSe/C nanofiber |
| CN112978685A (en) * | 2021-04-01 | 2021-06-18 | 陕西科技大学 | Pure-phase SnSe nano-particles and preparation method thereof |
| CN113005328A (en) * | 2021-02-23 | 2021-06-22 | 西安航空学院 | Tin-selenium-sulfur ternary alloy cathode material for sodium ion battery and preparation method and application thereof |
-
2008
- 2008-01-08 CN CNA2008100324185A patent/CN101214932A/en active Pending
Cited By (20)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101412505B (en) * | 2008-09-05 | 2010-06-02 | 山东建筑大学 | Preparation of high-purity tin diselenide nano-plate |
| CN101585518B (en) * | 2009-06-26 | 2011-03-30 | 上海大学 | Method for fast synthesizing powder of stannum selenide quanta dots |
| CN101920942A (en) * | 2010-09-20 | 2010-12-22 | 东华大学 | Method for controlling synthesis of zinc selenide multi-morphological nano material |
| CN101920942B (en) * | 2010-09-20 | 2012-02-15 | 东华大学 | Method for controlling synthesis of zinc selenide multi-morphological nano material |
| CN102897724A (en) * | 2012-09-06 | 2013-01-30 | 江苏大学 | Tin selenide nano-flowers and preparation method thereof |
| CN102897724B (en) * | 2012-09-06 | 2014-08-20 | 江苏大学 | Tin selenide nano-flowers and preparation method thereof |
| CN104692342B (en) * | 2015-02-17 | 2016-06-29 | 吉林大学 | A kind of preparation method of Tin monoselenide. nanosphere |
| CN104692342A (en) * | 2015-02-17 | 2015-06-10 | 吉林大学 | Preparation method of stannous selenide nanospheres |
| CN104692341A (en) * | 2015-02-17 | 2015-06-10 | 吉林大学 | SnSe square nanosheets and preparation method thereof |
| CN104692341B (en) * | 2015-02-17 | 2016-06-22 | 吉林大学 | A kind of Tin monoselenide. square nanometer sheet and preparation method thereof |
| CN104692343A (en) * | 2015-03-17 | 2015-06-10 | 福州大学 | Tin selenide nano material, preparation method and application thereof |
| CN104831362A (en) * | 2015-06-08 | 2015-08-12 | 广东工业大学 | Method for preparing tin selenide single-crystal nano-belt |
| CN105032451A (en) * | 2015-08-03 | 2015-11-11 | 广东工业大学 | Application of tin selenide nanometer material in photocatalysis aspect |
| CN106744727A (en) * | 2016-11-28 | 2017-05-31 | 福建师范大学 | Screw dislocation drives the preparation method of growth spiral type stratiform stannic selenide nanometer sheet |
| CN107381514A (en) * | 2017-08-09 | 2017-11-24 | 同济大学 | A kind of method of microwave radiation technology Fast back-projection algorithm stannic selenide nanometer sheet |
| CN107381514B (en) * | 2017-08-09 | 2019-10-18 | 同济大学 | A kind of method of microwave-assisted rapid synthesis stannic selenide nanometer sheet |
| CN109811428A (en) * | 2019-01-31 | 2019-05-28 | 湘潭大学 | A kind of electrostatic spinning preparation method of flexibility SnSe/C nanofiber |
| CN113005328A (en) * | 2021-02-23 | 2021-06-22 | 西安航空学院 | Tin-selenium-sulfur ternary alloy cathode material for sodium ion battery and preparation method and application thereof |
| CN113005328B (en) * | 2021-02-23 | 2021-12-07 | 西安航空学院 | Tin-selenium-sulfur ternary alloy cathode material for sodium ion battery and preparation method and application thereof |
| CN112978685A (en) * | 2021-04-01 | 2021-06-18 | 陕西科技大学 | Pure-phase SnSe nano-particles and preparation method thereof |
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Open date: 20080709 |