CN102040201A - Solvothermal controllable method for preparing ZnSe and ZnTe nano materials - Google Patents
Solvothermal controllable method for preparing ZnSe and ZnTe nano materials Download PDFInfo
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- CN102040201A CN102040201A CN 201010532909 CN201010532909A CN102040201A CN 102040201 A CN102040201 A CN 102040201A CN 201010532909 CN201010532909 CN 201010532909 CN 201010532909 A CN201010532909 A CN 201010532909A CN 102040201 A CN102040201 A CN 102040201A
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Abstract
The invention discloses a solvothermal controllable method for preparing ZnSe and ZnTe nano materials. The method comprises the following steps of: placing a Se source or Te source of an analytical reagent in an polytetrafluoroethylene inner lining; adding an ethanolamine solvent to ensure that the solution is 80 percent based on the total volume of the polytetrafluoroethylene inner lining; performing magnetic stirring for several minutes; adding the Zn source of the analytical reagent again; performing magnetic stirring uniformly and then sealing a reaction kettle; and placing in a baking oven at the temperature of 200 DEG C and reacting for 24 hours, after completing the reaction, cleaning to obtain a product. The ZnSe and ZnTe nano materials with a blende or wurtzite structure can be controllably synthesized successfully in one step in the same system by changing the Se source or the Te source through a simple solvothermal method under the mild condition for the first time. The method has the characteristics of simplicity, low cost, high yield, high uniformity of products, high controllability, environment friendliness and easiness in popularization and is suitable for large-scale production.
Description
Technical field
The invention belongs to the preparation field of nano material, be specifically related to utilize solvent thermal technology prepared product mutually and all controlled ZnSe of pattern and the method for ZnTe nano material.
Background technology
ZnSe and ZnTe are subject to people's attention as important broad-band gap II-VI family semiconductor material always, in fields such as photoelectric device, biosensor, photoelectrocatalysis, solar energy materialss wide application prospect are arranged.ZnSe and ZnTe (energy gap is respectively 2.7ev and 2.26eV) have broad-band gap, directly are with transition, and advantage such as can work under hot conditions can be used for making nonlinear optical electrical part, bluish-green laser device, photodetector and nuclear radiation detector etc.And the ZnSe of nanostructure and ZnTe material have the specific performance that does not possess as many macroscopic material such as small-size effect, surface effects, quantum size effect, macro quanta tunnel effect and dielectric confinement effects, have broad application prospects in fields such as optics, electronics, magnetics, but its concrete application is subjected to the restriction of factors such as thing phase, pattern and size.Therefore to the not jljl of ZnSe and ZnTe nano material mutually, the control of pattern and size is the focus of semiconductor material research always.The preparation method that ZnSe and ZnTe semiconductor nano material are commonly used mainly contains thermal evaporation, epitaxial growth method, electrodip process, chemical Vapor deposition process and hydrothermal method.Wherein, hydrothermal method is because technology is simple, and the preparation powder has characteristics such as high-purity, ultra-fine, that particle diameter is even, becomes the prefered method of preparation ZnSe and ZnSe nano material.
ZnSe and ZnTe generally have two kinds of crystalline structure, i.e. the zincblende lattce structure of cube phase and six sides wurtzite structure mutually, and the former is the cryostatic stabilization phase, the latter is the high-temperature stable phase.The report of synthetic different-shape zink sulphide ZnSe and ZnTe material is a lot, and actually rare about the report of wurtzite structure.Thing in the ZnSe nano material has certain progress mutually and aspect the morphology control research at present, P.Cozzoli Davide etc. has reported that with organic amine and organophosphorus be mixed solvent, utilize the hot route of high-temperature solvent to realize ZnSe nanometer colloid pattern and thing control mutually, consult the 1298th page of the 17th the 6th phase of volume of Chem.Mater.2005 by the ratio that changes precursor; Li Jun equality adopts hydrothermal technique, with butylamine (BA) is the structure directing template, and ethylenediamine tetraacetic acid (EDTA) (EDTA) is a stablizer, by changing temperature of reaction or BA consumption, the synthetic pattern ZnSe nanometer sheet structure mutually controlled with thing consulted " chemical journal " and rolled up the 2340th page of the 23rd phase in 2006 the 64th; Yuval Golan etc. have synthesized cube and six sides ZnSe nanostructure mutually by changing stearylamine (ODA) and trioctyl phosphine oxide (TOPO) dentate solvent ratios thermolysis zinc acetate and selenourea, consult Langmuir and roll up the 766th page of the 2nd phase in 2007 years the 23rd; Juan Yang etc. has reported with the ratio of passing through to change both in triethyl tetramine (TETA) and the deionized water mixed solvent, realized the ZnSe nanostructure that pattern is mutually controlled with thing, consulted Materials Chemistryand Physics and rolled up the 205th page in 2009 the 115th.
The research report of ZnTe is rare than ZnSe, the report of especially rarely seen preparation wurtzite structure ZnTe nano material, employing chemical Vapor deposition processs such as Geng Baoyou have synthesized wurtzite ZnTe nano wire, consult J.Phys.Chem.C and roll up the 20308th page of the 51st phase in 2008 the 112nd.Have not yet to see the report that the solvent thermal condition prepares wurtzite ZnTe nano material.
Existing research work is at the thing phase of ZnSe or ZnTe nano material or the research of the single aspect of pattern mostly, and adopts comparatively complicated experimental implementation method, as using template and stablizer, changes the mixed solvent proportioning, use N
2Protection or mode such as after baking processing need control in many ways, and it is less to reach the research of pattern mutually about the thing of simple control ZnSe and ZnTe in same system.Up to now, do not see as yet in same system that a simple step control is synthetic to have the ZnSe of zink sulphide or wurtzite structure and a report of ZnTe nano material.
Summary of the invention
The objective of the invention is to explore the synthesising law and the mutually controlled research of thing of ZnSe and ZnTe material under the same system.The present invention successfully uses the simple solvent by the use of thermal means first under the condition of gentleness, is solvent with the thanomin, is the Zn source with zinc acetate or zinc chloride, by regulating Se source or Te source, the ZnSe and the ZnTe nano material of synthetic zink sulphide of step control or wurtzite structure.
The present invention realizes by following technological process:
Polytetrafluoroethyllining lining is put in 1mmol analytically pure Se source or Te source, added the thanomin solvent and make liquor capacity account for 80% of polytetrafluoroethyllining lining cumulative volume.Magnetic stirred for several minute adds the analytically pure Zn of 2mmol source again, continues magnetic and is stirred to even back sealed reactor, places 200 ℃ of baking ovens reactions 24 hours.Naturally cool to room temperature, collect cooled product, with deionized water and dehydrated alcohol repetitive scrubbing, 60 ℃ of dryings of vacuum obtain product.
Technology of the present invention is simple, is being solvent with the thanomin, and zinc acetate or zinc chloride are in the system in zinc source, by change selenium source and tellurium source realize to final product ZnSe and ZnTe thing mutually, the control of pattern and size.The present invention is implemented in synthetic ZnSe and the ZnTe nano material with zink sulphide or wurtzite structure of step control in the same system first.
Description of drawings
Fig. 1 is X-ray diffraction (XRD) collection of illustrative plates of embodiment 1 product.
Fig. 2 is scanning electronic microscope (SEM) picture of embodiment 1 product.
Fig. 3 is the XRD figure spectrum of embodiment 2 products.
Fig. 4 is the SEM picture of embodiment 2 products.
Fig. 5 is the XRD figure spectrum of embodiment 3 products.
Fig. 6 is the SEM picture of embodiment 3 products.
Fig. 7 is the XRD figure spectrum of embodiment 4 products.
Fig. 8 is the SEM picture of embodiment 4 products.
Embodiment
Embodiment 1
With the analytically pure Sodium Selenite (Na of 1mmol
2SeO
35H
2O) put into polytetrafluoroethyllining lining, add the thanomin solvent and make liquor capacity account for 80% of polytetrafluoroethyllining lining cumulative volume.Magnetic stirred for several minute adds the analytically pure zinc acetate of 2mmol (Zn (CH again
3COO)
22H
2O), continue magnetic and be stirred to even back sealed reactor, place 200 ℃ of baking oven reactions 24 hours.Naturally cool to room temperature, collect cooled product, with deionized water and dehydrated alcohol repetitive scrubbing, 60 ℃ of dryings of vacuum obtain the tawny product.As shown in Figure 1, XRD result shows that product is cube ZnSe of phase zincblende lattce structure; SEM result shows that product is made up of the nanoparticle agglomerates of diameter about 100nm, as Fig. 2.
Embodiment 2
The analytically pure selenium powder of 1mmol (Se) is put into polytetrafluoroethyllining lining, add the thanomin solvent and make liquor capacity account for 80% of polytetrafluoroethyllining lining cumulative volume.Magnetic stirred for several minute adds the analytically pure zinc acetate of 2mmol (Zn (CH again
3COO)
22H
2O), continue magnetic and be stirred to even back sealed reactor, place 200 ℃ of baking oven reactions 24 hours.Naturally cool to room temperature, collect cooled product, with deionized water and dehydrated alcohol repetitive scrubbing, 60 ℃ of dryings of vacuum obtain the tawny product.XRD result shows that product is the ZnSe of six side's phase wurtzite structures, as Fig. 3; SEM result shows that product is made up of the nanometer sheet of the about 100nm of thickness, as shown in Figure 4.
Embodiment 3
With the analytically pure sodium tellurite (Na of 1mmol
2TeO
3) put into polytetrafluoroethyllining lining, add the thanomin solvent and make liquor capacity account for 80% of polytetrafluoroethyllining lining cumulative volume.Magnetic stirred for several minute adds the analytically pure zinc acetate of 2mmol (Zn (CH again
3COO)
22H
2O), continue magnetic and be stirred to even back sealed reactor, place 200 ℃ of baking oven reactions 24 hours.Naturally cool to room temperature, collect cooled product, with deionized water and dehydrated alcohol repetitive scrubbing, 60 ℃ of dryings of vacuum obtain the black product.XRD result shows that product is cube ZnTe of phase zincblende lattce structure, as Fig. 5; SEM result shows that product is made up of the nanoparticle agglomerates of diameter about 100nm, as Fig. 6.
Embodiment 4
The analytically pure tellurium powder of 1mmol (Te) is put into polytetrafluoroethyllining lining, add the thanomin solvent and make liquor capacity account for 80% of polytetrafluoroethyllining lining cumulative volume.Magnetic stirred for several minute adds the analytically pure zinc acetate of 2mmol (Zn (CH again
3COO)
22H
2O), continue magnetic and be stirred to even back sealed reactor, place 200 ℃ of baking oven reactions 24 hours.Naturally cool to room temperature, collect cooled product, with deionized water and dehydrated alcohol repetitive scrubbing, 60 ℃ of dryings of vacuum obtain the black product.XRD result shows that product is the ZnTe of six side's phase wurtzite structures, as Fig. 7; SEM result shows that product is made up of the nanometer sheet of the about 100nm of thickness, as shown in Figure 8.
Embodiment 5
With the analytically pure Sodium Selenite (Na of 1mmol
2SeO
35H
2O) put into polytetrafluoroethyllining lining, add the thanomin solvent and make liquor capacity account for 80% of polytetrafluoroethyllining lining cumulative volume.Magnetic stirred for several minute adds the analytically pure zinc chloride (ZnCl of 2mmol again
2), continue magnetic and be stirred to even back sealed reactor, place 200 ℃ of baking oven reactions 24 hours.Naturally cool to room temperature, collect cooled product, with deionized water and dehydrated alcohol repetitive scrubbing, 60 ℃ of dryings of vacuum obtain the tawny product.Analysis is shown as the ZnSe nano particle of zincblende lattce structure.
Embodiment 6
The analytically pure selenium powder of 1mmol (Se) is put into polytetrafluoroethyllining lining, add the thanomin solvent and make liquor capacity account for 80% of polytetrafluoroethyllining lining cumulative volume.Magnetic stirred for several minute adds the analytically pure zinc chloride (ZnCl of 2mmol again
2), continue magnetic and be stirred to even back sealed reactor, place 200 ℃ of baking oven reactions 24 hours.Naturally cool to room temperature, collect cooled product, with deionized water and dehydrated alcohol repetitive scrubbing, 60 ℃ of dryings of vacuum obtain the tawny product.Analysis is shown as the ZnSe nanometer sheet of wurtzite structure.
Embodiment 7
With the analytically pure sodium tellurite (Na of 1mmol
2TeO
3) put into polytetrafluoroethyllining lining, add the thanomin solvent and make liquor capacity account for 80% of polytetrafluoroethyllining lining cumulative volume.Magnetic stirred for several minute adds the analytically pure zinc chloride (ZnCl of 2mmol again
2), continue magnetic and be stirred to even back sealed reactor, place 200 ℃ of baking oven reactions 24 hours.Naturally cool to room temperature, collect cooled product, with deionized water and dehydrated alcohol repetitive scrubbing, 60 ℃ of dryings of vacuum obtain the black product.Analysis is shown as the ZnTe nano particle of zincblende lattce structure.
Embodiment 8
The analytically pure tellurium powder of 1mmol (Te) is put into polytetrafluoroethyllining lining, add the thanomin solvent and make liquor capacity account for 80% of polytetrafluoroethyllining lining cumulative volume.Magnetic stirred for several minute adds the analytically pure zinc chloride (ZnCl of 2mmol again
2), continue magnetic and be stirred to even back sealed reactor, place 200 ℃ of baking oven reactions 24 hours.Naturally cool to room temperature, collect cooled product, with deionized water and dehydrated alcohol repetitive scrubbing, 60 ℃ of dryings of vacuum obtain the black product.Analysis is shown as the ZnTe nanometer sheet of wurtzite structure.
Claims (9)
1. controlled method for preparing ZnSe and ZnTe nano material of solvent thermal, it is characterized in that realizing: polytetrafluoroethyllining lining is put in 1mmol analytically pure Se source or Te source, added the thanomin solvent and make liquor capacity account for 80% of polytetrafluoroethyllining lining cumulative volume by following technological process.Magnetic stirred for several minute adds the analytically pure Zn of 2mmol source again, continues magnetic and is stirred to even back sealed reactor, places 200 ℃ of baking ovens reactions 24 hours.Naturally cool to room temperature, collect cooled product, with deionized water and dehydrated alcohol repetitive scrubbing, 60 ℃ of dryings of vacuum obtain product.
2. the controlled method for preparing ZnSe and ZnTe nano material of a kind of solvent thermal as claimed in claim 1 is characterized in that described solvent is a thanomin.
3. the controlled method for preparing ZnSe and ZnTe nano material of a kind of solvent thermal as claimed in claim 1 is characterized in that described Se source or Te source are selenium powder (Se), Sodium Selenite (Na
2SeO
35H
2O), tellurium powder (Te) and sodium tellurite (Na
2TeO
3).
4. the controlled method for preparing ZnSe and ZnTe nano material of a kind of solvent thermal as claimed in claim 1 is characterized in that described Zn source is zinc acetate (Zn (CH
3COO)
22H
2O) and zinc chloride (ZnCl
2).
5. the controlled method for preparing ZnSe and ZnTe nano material of a kind of solvent thermal as claimed in claim 1 is characterized in that described Se source or Te source and Zn source mol ratio are 1: 2.
6. the controlled method for preparing ZnSe and ZnTe nano material of a kind of solvent thermal as claimed in claim 1 is characterized in that described solvent compactedness is 80%.
7. the controlled method for preparing ZnSe and ZnTe nano material of a kind of solvent thermal as claimed in claim 1 is characterized in that the described time is 24 hours.
8. the controlled method for preparing ZnSe and ZnTe nano material of a kind of solvent thermal as claimed in claim 1 is characterized in that described temperature is 200 ℃.
9. the controlled method for preparing ZnSe and ZnTe nano material of a kind of solvent thermal as claimed in claim 1 is characterized in that described reaction vessel is the tetrafluoroethylene hydrothermal reaction kettle, can expand in the closed container of other high temperature high voltage resistants.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103991850A (en) * | 2014-05-14 | 2014-08-20 | 新疆大学 | Preparation method of S-doped ZnTe |
| CN107572489A (en) * | 2017-08-07 | 2018-01-12 | 中国科学技术大学 | A kind of zinc selenide ultrathin nanometer band and prepare its anion exchange methods |
| CN108365211A (en) * | 2018-04-20 | 2018-08-03 | 合肥工业大学 | A kind of preparation method of nitrogen-doped carbon cladding zinc telluridse nano wire and its application as anode material of lithium-ion battery |
| CN108493285A (en) * | 2018-05-15 | 2018-09-04 | 华南理工大学 | A kind of cadmium telluride nano crystal solar cell and preparation method thereof based on environment-friendly type, the nanocrystalline buffer layer of nontoxic wide band gap semiconducter |
| CN112047310A (en) * | 2018-09-15 | 2020-12-08 | 东莞理工学院 | Preparation method of Ag-doped ZnTe semiconductor nano material |
-
2010
- 2010-11-05 CN CN 201010532909 patent/CN102040201A/en active Pending
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103991850A (en) * | 2014-05-14 | 2014-08-20 | 新疆大学 | Preparation method of S-doped ZnTe |
| CN103991850B (en) * | 2014-05-14 | 2016-10-26 | 新疆大学 | A kind of preparation method of the ZnTe of the S that adulterates |
| CN107572489A (en) * | 2017-08-07 | 2018-01-12 | 中国科学技术大学 | A kind of zinc selenide ultrathin nanometer band and prepare its anion exchange methods |
| CN107572489B (en) * | 2017-08-07 | 2020-01-03 | 中国科学技术大学 | Zinc selenide ultrathin nanobelt and anion exchange method for preparing same |
| CN108365211A (en) * | 2018-04-20 | 2018-08-03 | 合肥工业大学 | A kind of preparation method of nitrogen-doped carbon cladding zinc telluridse nano wire and its application as anode material of lithium-ion battery |
| CN108493285A (en) * | 2018-05-15 | 2018-09-04 | 华南理工大学 | A kind of cadmium telluride nano crystal solar cell and preparation method thereof based on environment-friendly type, the nanocrystalline buffer layer of nontoxic wide band gap semiconducter |
| CN112047310A (en) * | 2018-09-15 | 2020-12-08 | 东莞理工学院 | Preparation method of Ag-doped ZnTe semiconductor nano material |
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Application publication date: 20110504 |