CN103754836B - Prepare the method for high chemical reactivity tellurium colloid solution and telluride nano-material - Google Patents
Prepare the method for high chemical reactivity tellurium colloid solution and telluride nano-material Download PDFInfo
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- CN103754836B CN103754836B CN201410025377.2A CN201410025377A CN103754836B CN 103754836 B CN103754836 B CN 103754836B CN 201410025377 A CN201410025377 A CN 201410025377A CN 103754836 B CN103754836 B CN 103754836B
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Abstract
The invention discloses a kind of method preparing high chemical reactivity tellurium colloid solution and telluride nano-material, utilize pulse laser corrode placement simple substance tellurium target in deionized water, obtain corresponding tellurium colloid solution, tellurium nanoparticle size is little, be evenly distributed, surface " cleaning ", with it for precursors, carry out chemical reaction with the salts solution of metal ion, can successfully obtain corresponding telluride nano-material.
Description
Technical field
The present invention relates to one and prepare tellurium colloid solution and telluride nano-material technology, particularly relate to a kind of method preparing high chemical reactivity tellurium colloid solution and telluride nano-material.
Background technology
Tellurium belongs to VIA race, and be the very typical metalloid element of one, be also a kind of important narrow bandgap semiconductor material simultaneously.Because tellurium has physics, the chemical property of a series of uniqueness, such as: nonlinear optical response, piezoelectricity, catalytic activity, photoconductivity and thermoelectricity capability, therefore in a lot of field, all there is potential application prospect.The metallic compound of tellurium, as CdTe, ZnTe, PbTe etc., because having wider energy gap, there is very important application in fields such as light emitting semiconductor device, thermoelectric material, nonlinear optical material, electrooptical device, light-sensitive sensors material, photocatalyst material, hydrogen storage materials.The control synthesis of these telluride nano-materials and related property modulation thereof become the focus of research both at home and abroad.Exploration about telluride nano-material preparation method enjoys the concern of people, reports that more preparation method is with tellurium powder, sodium tellurite (Na in current pertinent literature
2teO
3) or tellurium dioxide (TeO
2) be tellurium source, after reductive agent reduction, add tensio-active agent and its pH is regulated, as the precursor solution of tellurium, then with metal ion (Ag
+, Cd
2+deng) salts solution carry out reaction under different conditions and be prepared.To prepare cadmium telluride: add NaBH when preparing with tellurium powder
4, tellurium powder is reduced to NaHTe presoma, and then is injected in cadmium precursor solution.But the above-mentioned process preparing telluride is more loaded down with trivial details, will regulate, also need to add stablizer, tensio-active agent or tensio-active agent in the solution after adding reductive agent to the pH value of solution.Then carry out hydrothermal treatment consists to the mixing solutions of presoma, the conditions such as reaction times, temperature of reaction and solution ph that are also noted that in hydrothermal treatment process are on the impact of product.
At least there is following shortcoming in above-mentioned prior art:
The stablizer added, tensio-active agent or surface-modifying agent are organism, make the inevitable absorbed portion organic agent molecule in the surface of the telluride nano-material obtained, and are difficult to clean up the telluride nano-material obtaining surface cleaning.
Summary of the invention
The object of this invention is to provide a kind of method preparing high chemical reactivity tellurium colloid solution and telluride nano-material, tellurium nanoparticle size prepared by the method be little, be evenly distributed, surface " cleaning ".
The object of the invention is to be achieved through the following technical solutions:
The method of preparation of the present invention high chemical reactivity tellurium colloid solution, utilizes pulse laser corrode placement simple substance tellurium target in deionized water, obtains corresponding tellurium colloid solution.
The method preparing telluride nano-material of the present invention, with above-mentioned prepared high chemical reactivity tellurium colloid solution for precursors, carries out chemical reaction with the salts solution of metal ion, can prepare corresponding telluride nano-material.
As seen from the above technical solution provided by the invention, the method of the preparation that the embodiment of the present invention provides high chemical reactivity tellurium colloid solution and telluride nano-material, owing to utilizing pulse laser corrode placement simple substance tellurium target in deionized water, obtain corresponding tellurium colloid solution, tellurium nanoparticle size is little, be evenly distributed, surface " cleaning ", with it for precursors, carry out chemical reaction with the salts solution of metal ion, have successfully been obtained corresponding telluride nano-material.
Accompanying drawing explanation
The schematic flow sheet of the method for the preparation high chemical reactivity tellurium colloid solution that Fig. 1 provides for the embodiment of the present invention and telluride nano-material.
Fig. 2 a is the TEM photo of tellurium nano particle in the tellurium colloid solution prepared of the embodiment of the present invention;
Fig. 2 b is the HRTEM photo of tellurium nano particle in the tellurium colloid solution prepared of the embodiment of the present invention;
Fig. 3 is the XRD figure picture of tellurium nano particle in the tellurium colloid solution prepared of the embodiment of the present invention;
Fig. 4 is the ultraviolet-visible light photoabsorption image of tellurium colloid solution prepared by the embodiment of the present invention;
Fig. 5 a is Ag prepared by the embodiment of the present invention
2the SEM photo of Te nanometer ball;
Fig. 5 b is Ag prepared by the embodiment of the present invention
2the XRD figure picture of Te nanometer ball.
Embodiment
To be described in further detail the embodiment of the present invention below.
The method of preparation of the present invention high chemical reactivity tellurium colloid solution, its preferably embodiment be:
Utilize pulse laser corrode placement simple substance tellurium target in deionized water, obtain corresponding tellurium colloid solution.
The purity of described simple substance tellurium target is more than or equal to 99.999%.
The wavelength of described pulse laser is 1064nm, energy is 80mJ/pulse, the time of corrode simple substance tellurium target is 5 minutes.
Described pulse laser adopts Nd:YAG pulsed laser to obtain.
In described corrosion process, rotate tellurium target and carry out laser ablation.
The method preparing telluride nano-material of the present invention, its preferably embodiment be:
With the high chemical reactivity tellurium colloid solution of above-mentioned preparation for precursors, carry out chemical reaction with the salts solution of metal ion, corresponding telluride nano-material can be prepared.
After described tellurium colloid solution mixes with the salts solution of metal ion, heating in water bath to 60 DEG C carries out isothermal reaction, can obtain the telluride nanometer ball of even size distribution.
Described telluride nano-material comprise following any one or more: Ag
2te, CuTe, CdTe, PbTe, ZnTe, Bi
2te
3, Sb
2te
3.
Described salts solution is nitrate solution.
The tellurium colloid solution of high reaction activity prepared by the present invention, the tellurium nano particle obtained by LAL technology have size little, be evenly distributed, the surface feature such as " cleaning ", with it for precursors, carry out chemical reaction with the salts solution of metal ion, have successfully been obtained corresponding telluride nano-material.
The present invention's a kind of tellurium colloid solution with high reaction activity that utilized liquid laser corrode (LAL) technology to prepare, and with it for precursors, by simple chemical reaction, obtain a series of telluride nano-material.In LAL process, utilize pulse laser corrode to place simple substance tellurium target in deionized water first, corresponding tellurium colloid solution can be obtained, and detailed thing has been carried out to it characterize mutually and Study on Microstructure.Compared with the tellurium colloid solution prepared with chemical process of the prior art, the tellurium colloid solution obtained by LAL technology has very high chemical reactivity, and tellurium nanoparticle size is wherein evenly distributed, surface " cleaning ", do not adsorb any organic compound, not easily coagulation.
Based on the high reaction activity of above-mentioned tellurium colloid solution, with it for precursors, with metal ion (such as Ag
+) salts solution under condition as mild as a dove, carry out chemical reaction, successfully can prepare corresponding telluride nano-material (such as Ag
2te).
Based on the above results, the present invention, by similar experimental technique, obtains CuTe, CdTe, PbTe, ZnTe, Bi
2te
3, Sb
2te
3etc. a series of telluride nano-material.The method reaction conditions adopting the tellurium colloid solution of high reaction activity to prepare telluride nano-material as precursors is gentle, and without the need to adding reductive agent, stablizer and tensio-active agent in reaction process, is the synthetic technology of an environmental protection.Proposition of the present invention is that the synthesis of telluride nano-material provides new approach and thinking, has also widened the application prospect of LAL technology in colloidal solution chemical reaction field simultaneously.
Specific embodiment:
To prepare silver telluride:
As shown in Figure 1, LAL technology is first utilized to prepare the tellurium colloid solution of high reaction activity, then by itself and a certain amount of Silver Nitrate (AgNO
3) solution mixes, heating in water bath to 60 DEG C, can obtain the silver telluride (Ag of even size distribution after reaction for some time
2te) nanometer ball.
The method utilizing LAL technology to prepare the tellurium colloid solution of high reaction activity is:
By purity be 99.999% tellurium simple substance target be placed in the container that 15ml deionized water is housed, (optical maser wavelength is 1064nm to adopt Nd:YAG pulsed laser, energy is 80mJ/pulse) corrode tellurium simple substance target 5 minutes, adopt in the process of corrode and rotate tellurium target and carry out laser ablation (adopting rotary target corrode can obtain the colloidal solution of evenly tiny nano particle).
The Ag of preparation even particle size distribution
2the method of Te nanometer ball is:
The Te colloidal solution getting preparation in three mouthfuls of round-bottomed flasks, by Ag
2nO
3solution is added drop-wise to wherein.The water bath that three mouthfuls of round-bottomed flasks are placed in 60 DEG C is carried out constant temperature process, after reaction for some time, successfully can prepare the Ag of even particle size distribution
2te nanometer ball.
Fig. 2 a is the TEM photo of tellurium nano particle in tellurium colloid solution, can find out that the tellurium nano particle diameter in tellurium colloid is evenly distributed, at about 15nm.Fig. 2 b is the HRTEM photo of tellurium nano particle in tellurium colloid solution, can show that the spacing of tellurium nano particle in Fig. 2 b is 0.383nm by measuring, consistent with the spacing of the crystal face (100) of six side's phase telluriums.
Fig. 3 is the XRD figure picture of tellurium nano particle in tellurium colloid solution, the diffraction peak in figure is contrasted with standard x RD database, corresponding with JCPDS, CardNO.78-2312.Tellurium in the tellurium colloid solution prepared as seen from Figure 3 exists with six side's phase tellurium simple substance forms, and spacer is P3121, and lattice parameter is
diffraction peak stronger in XRD figure appears at 2 θ=23.022 °, 27.552 °, 38.250 °, 40.442 °, 43.339 ° and 49.635 °, corresponding with crystal face (100), (101), (012), (110), (111) and (021) respectively.
Fig. 4 is the ultraviolet-visible light photoabsorption image of tellurium colloid solution, can be found out that by the absorption peak in figure the energy gap of tellurium nano particle in the tellurium colloid solution prepared by LAL technology is about 4.05eV, and block tellurium is low-gap semiconductor, energy gap is 0.35eV.The tellurium nano particle prepared by LAL technology shows character different with block tellurium, and this is due to quantum size effect, makes the band gap broadening of the tellurium nano particle of nano-scale.
Fig. 5 a, Fig. 5 b are respectively the Ag prepared by aforesaid method
2the SEM photo of Te nanometer ball and XRD figure picture.Tellurium colloid solution and AgNO can be found out by Fig. 5 a
3solution carries out reacting the nanometer ball that rear generation is evenly distributed.By the Ag that Fig. 5 b is preparation
2the XRD figure picture of Te nanometer ball, contrasts the diffraction peak in figure with standard x RD database, corresponding with JCPDS, CardNO.81-1985.The silver telluride of characterization result display preparation is monoclinic phase, and space group is P21/c, and lattice parameter is
α=90 °, β=90 °, γ=124.16 °.
Above-described embodiment as the tellurium precursor solution preparing telluride, has successfully prepared Ag by high reaction activity tellurium colloid
2te nanometer ball.This is exploration new in telluride preparation method, utilizes TeO before instead of
2, Na
2teO
3or tellurium powder is as the method in tellurium source, decrease the application of the reagent such as reductive agent, stablizer and tensio-active agent.
The above; be only the present invention's preferably embodiment, but protection scope of the present invention is not limited thereto, is anyly familiar with those skilled in the art in the technical scope that the present invention discloses; the change that can expect easily or replacement, all should be encompassed within protection scope of the present invention.Therefore, protection scope of the present invention should be as the criterion with the protection domain of claims.
Claims (2)
1. prepare a method for telluride nano-material, it is characterized in that, with high chemical reactivity tellurium colloid solution for precursors, carry out chemical reaction with the salts solution of metal ion, corresponding telluride nano-material can be prepared;
After described high chemical reactivity tellurium colloid solution mixes with the salts solution of metal ion, heating in water bath to 60 DEG C carries out isothermal reaction, can obtain the telluride nanometer ball of even size distribution;
Described high chemical reactivity tellurium colloid solution is prepared by the following method:
Utilize pulse laser corrode placement simple substance tellurium target in deionized water, obtain corresponding tellurium colloid solution, in corrosion process, rotate tellurium target and carry out laser ablation.
2. the method preparing telluride nano-material according to claim 1, is characterized in that, described telluride nano-material comprise following any one or more: Ag
2te, CuTe, CdTe, PbTe, ZnTe, Bi
2te
3, Sb
2te
3.
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| WO2011052279A1 (en) * | 2009-10-28 | 2011-05-05 | 国立大学法人筑波大学 | Phase change device having phase change recording film, and phase change switching method for phase change recording film |
| US8957299B2 (en) * | 2011-01-24 | 2015-02-17 | Samsung Electronics Co., Ltd. | Thermoelectric material including nano-inclusions, thermoelectric module and thermoelectric apparatus including the same |
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| CN1394882A (en) * | 2002-08-10 | 2003-02-05 | 吉林大学 | Preparation method of CdTe nano crystal transparent polymer body phase material with high visible luminescent efficiency |
| CN101327916A (en) * | 2008-07-17 | 2008-12-24 | 武汉理工大学 | Preparation of Bi2Te3 thermoelectric compound nanopowder |
| CN101913574A (en) * | 2010-07-08 | 2010-12-15 | 浙江大学 | Preparation method of cadmium telluride quantum dot |
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