CN103754836A - Method for preparing tellurium colloid solution with high chemical activity and telluride nanometer material - Google Patents

Method for preparing tellurium colloid solution with high chemical activity and telluride nanometer material Download PDF

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CN103754836A
CN103754836A CN201410025377.2A CN201410025377A CN103754836A CN 103754836 A CN103754836 A CN 103754836A CN 201410025377 A CN201410025377 A CN 201410025377A CN 103754836 A CN103754836 A CN 103754836A
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tellurium
solution
colloid solution
telluride
high chemical
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CN103754836B (en
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张峰通
刘俊
梁长浩
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Hefei Institutes of Physical Science of CAS
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Abstract

The invention discloses a method for preparing a tellurium colloid solution with high chemical activity and a telluride nanometer material. The method comprises the following steps: corroding an elementary tellurium target placed into deionized water by using pulse laser light to obtain a corresponding tellurium colloid solution; performing a chemical reaction on tellurium nanoparticles which are small in sizes, distributed uniformly, clean in surfaces and taken as a reaction precursor and a saline solution of metal ions to obtain a corresponding telluride nanometer material successfully.

Description

Prepare the method for high chemical reactivity tellurium colloid solution and telluride nano-material
Technical field
The present invention relates to one and prepare tellurium colloid solution and telluride nano-material technology, relate in particular to a kind of method of preparing high chemical reactivity tellurium colloid solution and telluride nano-material.
Background technology
Tellurium belongs to VIA family, is the very typical metalloid element of one, is also a kind of important narrow bandgap semiconductor material simultaneously.For example, because tellurium has physics, the chemical property of a series of uniquenesses: nonlinear optical response, piezoelectricity, catalytic activity, photoconductivity and thermoelectricity capability, therefore all have potential application prospect in a lot of fields.The metallic compound of tellurium, as CdTe, ZnTe, PbTe etc., because thering is wider energy gap, in fields such as light emitting semiconductor device, thermoelectric material, nonlinear optical material, electrooptical device, light-sensitive sensors material, photocatalyst material, hydrogen storage materials, there is very important application.The control of these telluride nano-materials is synthesized and related property is modulated the focus that becomes domestic and international research.About telluride nano-material preparation method's exploration, enjoy people's concern, in pertinent literature, report that more preparation method is with tellurium powder, sodium tellurite (Na at present 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 under different conditions, react and be prepared.To prepare cadmium telluride as example: 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 of preparing telluride is more loaded down with trivial details, adding after reductive agent and will regulating the pH value of solution, also need in solution, add stablizer, tensio-active agent or tensio-active agent.Then the mixing solutions of presoma is carried out to hydrothermal treatment consists, in hydrothermal treatment consists process, be also noted that the impacts of condition on product such as reaction times, temperature of reaction and pH.
At least there is following shortcoming in above-mentioned prior art:
The stablizer, tensio-active agent or the surface-modifying agent that add are organism, make the surface inevitable absorbed portion organic reagent molecule of the telluride nano-material making, and are difficult to clean up the telluride nano-material that obtains surface cleaning.
Summary of the invention
The object of this invention is to provide a kind of method of preparing high chemical reactivity tellurium colloid solution and telluride nano-material, tellurium nanoparticle size prepared by the method is little, be evenly distributed, surface " cleaning ".
The object of the invention is to be achieved through the following technical solutions:
The method of the high chemical reactivity tellurium colloid of preparation of the present invention solution, utilizes pulse laser corrode to be placed on the simple substance tellurium target in deionized water, obtains corresponding tellurium colloid solution.
The method of preparing telluride nano-material of the present invention, take above-mentioned prepared high chemical reactivity tellurium colloid solution as 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 preparation high chemical reactivity tellurium colloid solution that the embodiment of the present invention provides and the method for telluride nano-material, owing to utilizing pulse laser corrode to be placed on the simple substance tellurium target in deionized water, obtain corresponding tellurium colloid solution, tellurium nanoparticle size is little, be evenly distributed, surface " cleaning ", take it as precursors, carry out chemical reaction with the salts solution of metal ion, successfully obtained corresponding telluride nano-material.
Accompanying drawing explanation
The schematic flow sheet of the preparation high chemical reactivity tellurium colloid solution that Fig. 1 provides for the embodiment of the present invention and the method for 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 the tellurium colloid solution prepared of 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 the high chemical reactivity tellurium colloid of preparation of the present invention solution, its preferably embodiment be:
Utilize pulse laser corrode to be placed on the 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 that 1064nm, energy are that time of 80mJ/pulse, 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 while carry out laser ablation.
The method of preparing telluride nano-material of the present invention, its preferably embodiment be:
Take the high chemical reactivity tellurium colloid solution of above-mentioned preparation as precursors, carry out chemical reaction with the salts solution of metal ion, can prepare corresponding telluride nano-material.
After described tellurium colloid solution mixes with the salts solution of metal ion, heating in water bath to 60 ℃ 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 obtaining by LAL technology have size little, be evenly distributed, feature such as surface " cleaning " etc., take it as precursors, carry out chemical reaction with the salts solution of metal ion, successfully obtained corresponding telluride nano-material.
The present invention utilizes liquid laser corrode (LAL) technology to prepare a kind of tellurium colloid solution with high reaction activity, and take it as precursors, by simple chemical reaction, has obtained a series of telluride nano-material.In LAL process, utilize first pulse laser corrode to be placed on the simple substance tellurium target in deionized water, can obtain corresponding tellurium colloid solution, and it has been carried out to detailed thing characterize mutually and Study on Microstructure.The tellurium colloid solution phase comparison of preparing with chemical process of the prior art, the tellurium colloid solution obtaining by LAL technology has very high chemical reactivity, and tellurium nanoparticle size is wherein evenly distributed, surface " cleaning ", do not adsorb any organic compound, be difficult for coagulation.
Based on the high reaction activity of above-mentioned tellurium colloid solution, take it as precursors, for example, with metal ion (Ag +) salts solution under condition as mild as a dove, carry out chemical reaction, can successfully prepare corresponding telluride nano-material (for example 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-materials.Adopt the tellurium colloid solution of high reaction activity as precursors, to prepare the method reaction conditions gentleness of telluride nano-material, and in reaction process without adding reductive agent, stablizer and tensio-active agent, be the synthetic technology of an environmental protection.Proposition of the present invention is telluride nano-material syntheticly 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 example:
As shown in Figure 1, first utilize LAL technology 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 ℃, can obtain the silver telluride (Ag of even size distribution after reaction for some time 2te) nanometer ball.
The method of utilizing LAL technology to prepare the tellurium colloid solution of high reaction activity is:
The tellurium simple substance target that is 99.999% by purity is 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, in the process of corrode, adopt rotation tellurium target to carry out laser ablation (adopting rotary target corrode can obtain the colloidal solution of evenly tiny nano particle).
The uniform Ag of preparation size distribution 2the method of Te nanometer ball is:
Get the Te colloidal solution of 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 to 60 ℃ carries out constant temperature processing, after reaction for some time, can successfully prepare the uniform Ag of 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, in 15nm left and right.Fig. 2 b is the HRTEM photo of tellurium nano particle in tellurium colloid solution, by measuring, can show that the spacing of tellurium nano particle in Fig. 2 b is 0.383nm, 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, and the diffraction peak in figure is contrasted with standard x RD database, and with JCPDS, Card NO.78-2312 is corresponding.Tellurium in the tellurium colloid solution of preparation is to exist with six side's phase tellurium simple substance forms as seen from Figure 3, and spacer is P3121, and lattice parameter is
Figure BDA0000459154930000041
in XRD figure, stronger diffraction peak 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, the energy gap that can be found out tellurium nano particle in the tellurium colloid solution of being prepared by LAL technology by the absorption peak in figure is about 4.05eV, and block tellurium is low-gap semiconductor, energy gap is 0.35eV.The tellurium nano particle of being prepared by LAL technology shows and the different character of 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 preparing by aforesaid method 2the SEM photo of Te nanometer ball and XRD figure picture.By Fig. 5 a, can find out tellurium colloid solution and AgNO 3solution reacts the nanometer ball that rear generation is evenly distributed.By Fig. 5 b, be the Ag of preparation 2the XRD figure picture of Te nanometer ball, contrasts the diffraction peak in figure with standard x RD database, with JCPDS, CardNO.81-1985 is corresponding.Characterization result shows that the silver telluride of preparation is monoclinic phase, and space group is P21/c, and lattice parameter is
Figure BDA0000459154930000042
α=90 °, β=90 °, γ=124.16 °.
Above-described embodiment as the tellurium precursor solution of preparing telluride, has successfully been prepared Ag by high reaction activity tellurium colloid 2te nanometer ball.This is exploration new in telluride preparation method, utilizes TeO before having substituted 2, Na 2teO 3or tellurium powder is as the method in tellurium source, has reduced the application of the reagent such as reductive agent, stablizer and tensio-active agent.
The above; only for preferably embodiment of the present invention, but protection scope of the present invention is not limited to this, is anyly familiar with in technical scope that those skilled in the art disclose in the present invention; the variation that can expect easily or replacement, within all should being encompassed in 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 (5)

1. a method of preparing high chemical reactivity tellurium colloid solution, is characterized in that, utilizes pulse laser corrode to be placed on the simple substance tellurium target in deionized water, obtains corresponding tellurium colloid solution.
2. the method for the high chemical reactivity tellurium colloid of preparation according to claim 1 solution, is characterized in that, in described corrosion process, rotates tellurium target while carries out laser ablation.
3. prepare the method for telluride nano-material for one kind, it is characterized in that, take the prepared high chemical reactivity tellurium colloid solution of claim 1 or 2 as precursors, carry out chemical reaction with the salts solution of metal ion, can prepare corresponding telluride nano-material.
4. the method for preparing telluride nano-material according to claim 3, it is characterized in that, after described tellurium colloid solution mixes with the salts solution of metal ion, heating in water bath to 60 ℃ carries out isothermal reaction, can obtain the telluride nanometer ball of even size distribution.
5. the method for preparing telluride nano-material according to claim 4, 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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