CN101798069B - Method for preparing rope-form tellurium nanocrystals - Google Patents
Method for preparing rope-form tellurium nanocrystals Download PDFInfo
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- CN101798069B CN101798069B CN2010101229876A CN201010122987A CN101798069B CN 101798069 B CN101798069 B CN 101798069B CN 2010101229876 A CN2010101229876 A CN 2010101229876A CN 201010122987 A CN201010122987 A CN 201010122987A CN 101798069 B CN101798069 B CN 101798069B
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Abstract
The invention relates to a method for preparing rope-form tellurium nanocrystals. The tellurium nanowires prepared by the conventional method have smooth surfaces. The method comprises the following steps: dissolving A grams of telluric acid and (0.5-2)A grams of mercapto compound in (0.5-1)A liters of mixed solvent, and adding (20-60)A grams of reducing agent; performing hydrothermal reaction ina hydrothermal reaction kettle at the temperature of between 100 and 140DEG C for 12 to 48 hours; after the reaction is finished, performing centrifugal separation on reactants to obtain a solid product; and washing the solid product by using distilled water and ethanol in turn, and drying to obtain black solid powder, namely the rope-form hexagonal tellurium nanocrystals. The method has the advantages of simple production process; and the prepared hexagonal tellurium nanocrystals are in a rope form, and have good uniformity.
Description
Technical field
The invention belongs to field of nanometer technology, relate to a kind of six side's phase preparing tellurium nanocrystals of rope-like constructed.
Background technology
Nano material is owing to the electronics confinement effect thereby show the specific physique different with the body phase material of same composition and receive much concern.Especially the character of nano material, not only relevant with its composition, size, also close getting in touch arranged with its pattern, therefore, can regulate its physicochemical property through the pattern of control nanocrystal.
Tellurium is a kind of semi-conductor with low energy gap width (0.35eV), because its character with many excellences attracts people's very big concern, is widely used as thermoelectric material, piezoelectric, light-guide material and catalytic material etc.In order to obtain the better application characteristic, people have carried out the preparation research of different-shape tellurium nanocrystals.Zhu Ying-Jie etc. are media with the ionic liquid, adopt the microwave-assisted method to prepare the single crystal tellurium nano wire [Angew.Chem.Int.Ed.2004,43,1410-1414] of surface smoothing; It is leg-of-mutton tellurium nanotube [J.Phys.Chem.B, 2006,110 (2) that a kind of simple and easy physics aerosol methods of employing such as Bongsoo Kim make the cross section; 791-795], Qian Yitai adopts the gamma-rays method to obtain ultra-fine aciculiform tellurium nano particle [J.Mater.Sci.Lett., 1996; 15,1700-1701], C.N.R.Rao etc. sow the solution process certainly through one; With tellurium powder and Peng Qinghuana is that raw material has made the tellurium nano-wire and the tellurium nanocrystals of other different-shape on a small quantity, comprises featheriness, banded and Y shape [J.Mater.Chem.; 2004,14,2530-2535].In addition; Shi Wensheng adopts the electrificationization deposition technique to prepare even tellurium nanotube [Crystal Growth & Design, 2009,9 (2); 663-666], a kind of simple fast method of inventions such as Zhu person of outstanding talent makes the tellurium nano-wire [CN1301346C] of surface smoothing.
Summary of the invention
The purpose of this invention is to provide a kind of method for preparing rope-form tellurium nanocrystals.
For realizing the foregoing invention purpose, the present invention adopts following technical scheme:
A is restrained positive telluric acid and (0.5～2) A gram sulfhydryl compound be dissolved in (0.5～1) A and rise in the mixed solvent, add (20～60) A then and restrain reductive agent; In hydrothermal reaction kettle, carry out hydro-thermal reaction, temperature of reaction is 100～140 ℃, and the reaction times is 12～48 hours; Reaction is carried out spinning with reactant after finishing, and obtains solid product; Solid product is used zero(ppm) water and washing with alcohol successively, obtain the black solid powder after the drying, be i.e. rope form six side's phase tellurium nanocrystals.
Said sulfhydryl compound is 2 mercaptopropionic acid or mercaptoethanol;
Described mixed solvent is the mixture of water and quadrol, and wherein the volume percent of quadrol in mixed solvent is 10～80 (V/V%);
Described reductive agent is a Hydrazine Hydrate 80 or Peng Qinghuana.
The production technique of the inventive method is simple, and the six side's phase tellurium nanocrystals that make are the single nano wire with torsion structure, i.e. rope form, and this rope-form tellurium nanocrystals has homogeneity preferably.
Embodiment
Further specify the present invention below in conjunction with embodiment.
Embodiment 1
In capacity is 100 milliliters polytetrafluoroethyltank tank, inject 72 ml deionized water and 8 milliliters of quadrols, add 0.16 positive telluric acid of gram and 0.08 gram 2 mercaptopropionic acid then, add 3.2 grams, one Hydrazine Hydrate 80 after the dissolving again.Polytetrafluoroethyltank tank is put into not the steel autoclave and added lid may enclose as inner bag, place heated oven reaction 48 hours then, temperature keeps 100 ℃.React and finish back taking-up polytetrafluoroethyltank tank, reaction solution is carried out spinning go out solid product, fund-raising is with deionized water and washing with alcohol then, and getting the black solid powder after the drying is rope form six side's phase tellurium nanocrystals.
Embodiment 2
In capacity is 100 milliliters polytetrafluoroethyltank tank, inject 16 ml deionized water and 64 milliliters of quadrols, add 0.08 positive telluric acid of gram and 0.16 gram 2 mercaptopropionic acid then, add 4.8 gram Peng Qinghuanas after the dissolving again.Polytetrafluoroethyltank tank is put into not the steel autoclave and added lid may enclose as inner bag, place heated oven reaction 12 hours then, temperature keeps 140 ℃.React and finish back taking-up polytetrafluoroethyltank tank, reaction solution is carried out spinning go out solid product, fund-raising is with deionized water and washing with alcohol then, and getting the black solid powder after the drying is rope form six side's phase tellurium nanocrystals.
Embodiment 3
In capacity is 100 milliliters polytetrafluoroethyltank tank, inject 50 ml deionized water and 30 milliliters of quadrols, add 0.1 positive telluric acid of gram and 0.1 gram 2 mercaptopropionic acid then, add 4 grams, one Hydrazine Hydrate 80 after the dissolving again.Polytetrafluoroethyltank tank is put into not the steel autoclave and added lid may enclose as inner bag, place heated oven reaction 24 hours then, temperature keeps 120 ℃.React and finish back taking-up polytetrafluoroethyltank tank, reaction solution is carried out spinning go out solid product, fund-raising is with deionized water and washing with alcohol then, and getting the black solid powder after the drying is rope form six side's phase tellurium nanocrystals.
Embodiment 4
In capacity is 50 milliliters polytetrafluoroethyltank tank, inject 20 ml deionized water and 20 milliliters of quadrols, add 0.08 positive telluric acid of gram and 0.1 gram mercaptoethanol then, add 2.4 gram Peng Qinghuanas after the dissolving again.Polytetrafluoroethyltank tank is put into not the steel autoclave and added lid may enclose as inner bag, place heated oven reaction 36 hours then, temperature keeps 120 ℃.React and finish back taking-up polytetrafluoroethyltank tank, reaction solution is carried out spinning go out solid product, fund-raising is with deionized water and washing with alcohol then, and getting the black solid powder after the drying is rope form six side's phase tellurium nanocrystals.
Embodiment 5
In capacity is 100 milliliters polytetrafluoroethyltank tank, inject 44 ml deionized water and 36 milliliters of quadrols, add 0.1 positive telluric acid of gram and 0.15 gram mercaptoethanol then, add 3 grams, one Hydrazine Hydrate 80 after the dissolving again.Polytetrafluoroethyltank tank is put into not the steel autoclave and added lid may enclose as inner bag, place heated oven reaction 24 hours then, temperature keeps 130 ℃.React and finish back taking-up polytetrafluoroethyltank tank, reaction solution is carried out spinning go out solid product, fund-raising is with deionized water and washing with alcohol then, and getting the black solid powder after the drying is rope form six side's phase tellurium nanocrystals.
Claims (2)
1. method for preparing rope-form tellurium nanocrystals is characterized in that this method specifically:
A is restrained positive telluric acid and 0.5A～2A gram sulfhydryl compound to be dissolved in 0.5A～1A and to rise in the mixed solvent, add 20A～60A then and restrain reductive agent; In hydrothermal reaction kettle, carry out hydro-thermal reaction, temperature of reaction is 100～140 ℃, and the reaction times is 12～48 hours; Reaction is carried out spinning with reactant after finishing, and obtains solid product; Solid product is used zero(ppm) water and washing with alcohol successively, dry then, obtain six side's phase tellurium nanocrystals; The six side's phase tellurium nanocrystals that make are the single nano wire with torsion structure, i.e. rope form;
Described mixed solvent is the mixture of water and quadrol, and wherein the volume percent of quadrol in mixed solvent is 10～80V/V%;
Described reductive agent is a Hydrazine Hydrate 80 or Peng Qinghuana.
2. method for preparing rope-form tellurium nanocrystals as claimed in claim 1 is characterized in that: described sulfhydryl compound is 2 mercaptopropionic acid or mercaptoethanol.
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| Application Number | Priority Date | Filing Date | Title |
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| CN2010101229876A CN101798069B (en) | 2010-03-12 | 2010-03-12 | Method for preparing rope-form tellurium nanocrystals |
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| CN2010101229876A CN101798069B (en) | 2010-03-12 | 2010-03-12 | Method for preparing rope-form tellurium nanocrystals |
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| CN102583269A (en) * | 2012-03-30 | 2012-07-18 | 哈尔滨工业大学 | Needle-shaped monocrystal tellurium and preparation method thereof |
| RU2629679C1 (en) * | 2016-11-29 | 2017-08-31 | Акционерное общество "Производственное объединение "Электрохимический завод" | Method for elemental tellurium production |
| CN107827087B (en) * | 2017-12-24 | 2020-03-24 | 韩金玲 | Preparation method of regularly bent tellurium nanowires |
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| WO2007051481A2 (en) * | 2005-11-02 | 2007-05-10 | Jozef Stefan Institute | Use of quasi-one-dimensional polymers based on the metal-chalcogen-halogen system |
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