CN101920940A - Method for preparing tellurium nanocrystals - Google Patents
Method for preparing tellurium nanocrystals Download PDFInfo
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- CN101920940A CN101920940A CN 201010262202 CN201010262202A CN101920940A CN 101920940 A CN101920940 A CN 101920940A CN 201010262202 CN201010262202 CN 201010262202 CN 201010262202 A CN201010262202 A CN 201010262202A CN 101920940 A CN101920940 A CN 101920940A
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- tellurium
- telluric
- nanocrystals
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Abstract
The invention relates to a method for preparing tellurium nanocrystals. The conventional method cannot effectively control the morphologies of the tellurium nanocrystals. The method comprises the following steps of: preparing aqueous solution of tellurium acid according to the morphology required by the prepared tellurium nanocrystals; adding a reducing agent hydrazine monohydrate into the aqueous solution of the tellurium acid to form black suspension solution, and pouring into a hydrothermal reactor for hydrothermal reaction at the temperature of between 100 and 120 DEG C for 12 to 24 hours; and centrifuging to separate the reaction products, and washing and drying the solid product to obtain the tellurium nanocrystals. The morphologies of the tellurium nanocrystals can be controlled by changing the concentration of the aqueous solution of tellurium acid in the reaction system, so the nanocrystals in different morphologies such as nanoparticles, short nanorods and long nanorods can be respectively obtained. The method has the advantages of simple process and stable reaction system; and the obtained tellurium nanocrystals have better uniformity and the morphologies of the obtained tellurium nanocrystals can be effectively controlled.
Description
Technical field
The invention belongs to technical field of semiconductor, be specifically related to a kind of preparing tellurium nanocrystals.
Background technology
Nano material is because its unique light, electricity, magnetic, sensitivity and mechanical property, the field such as constructs at nano-device and has the potential application prospect, is subjected to various countries scientist's extensive concern day by day.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 by 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 of surface smoothing, 43,1410-1414], it is leg-of-mutton tellurium nanotube [J.Phys.Chem.B that a kind of simple and easy physics aerosol methods of employing such as Bongsoo Kim make the cross section, 2006,110 (2), 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 by one, with tellurium powder and sodium borohydride is that raw material has made the tellurium nano-wire and the tellurium nanocrystals of other different-shape on a small quantity, comprise 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 ﹠amp; 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.But the preparation of different-shape semi-conductor tellurium nanocrystals remains a challenging problem.
Summary of the invention
The purpose of this invention is to provide a kind of preparing tellurium nanocrystals.
The concrete steps of the inventive method are as follows:
1. positive telluric acid is dissolved in the water, the pattern configuration telluric aqueous acid required according to the tellurium nanocrystals of preparation, specifically:
Prepare the tellurium nanocrystals particle as need, then Pei Zhi telluric aqueous acid concentration is M
1, 4 * 10
-2Mol/L＜M
1≤ 6 * 10
-2Mol/L;
Prepare the tellurium nanometer stub that length is 100～200 nanometers as need, then Pei Zhi telluric aqueous acid concentration is M
2, 3 * 10
-2Mol/L≤M
2≤ 4 * 10
-2Mol/L;
Prepare the tellurium nanometer long rod of length greater than 200 nanometers as need, then Pei Zhi telluric aqueous acid concentration is M
3, 1 * 10
-2Mol/L≤M
3＜3 * 10
-2Mol/L;
2. reductive agent one hydrazine hydrate is joined in the telluric aqueous acid, form black suspension solution; The amount that every milliliter of telluric aqueous acid adds a hydrazine hydrate is 1～2 mmole;
3. black suspension solution is poured into and carried out hydro-thermal reaction in the hydrothermal reaction kettle, temperature of reaction is 100～120 ℃, and the reaction times is 12～24 hours;
4. after hydro-thermal reaction finishes, reactant is carried out centrifugation, obtain solid product; Solid product is used distilled water and washing with alcohol successively, obtain the black solid powder after the drying, be tellurium nanocrystals.
The inventive method can be controlled the pattern of tellurium nanocrystals by the concentration that changes telluric aqueous acid in the reaction system, can obtain the tellurium nanocrystals of different-shapes such as nano particle, short nanometer rod, long nanometer rod respectively.The inventive method technology is simple, and reaction system is stable, and the gained tellurium nanocrystals has homogeneity preferably, and can effectively control the pattern of gained tellurium nanocrystals.
Embodiment
Further specify the inventive method below in conjunction with embodiment.
Embodiment 1
Prepare spherical tellurium nanocrystals particle, concrete steps are:
(1) positive telluric acid is dissolved in the water, forming concentration is 6 * 10
-2The telluric aqueous acid of mol/L;
(2) hydrazine hydrate of 60 mmoles is joined in 40 milliliters the telluric aqueous acid, form black suspension solution;
(3) black suspension solution is poured in the hydrothermal reaction kettle, reacted 24 hours down at 100 ℃;
(4) after hydro-thermal reaction finishes, reactant is carried out centrifugation, obtain solid product; Solid product is used distilled water and washing with alcohol successively, obtain spherical tellurium nanocrystals particle after the drying.
Embodiment 2
Preparation olive shape tellurium nanocrystals particle, concrete steps are:
(1) positive telluric acid is dissolved in the water, forming concentration is 5 * 10
-2The telluric aqueous acid of mol/L;
(2) hydrazine hydrate of 80 mmoles is joined in 40 milliliters the telluric aqueous acid, form black suspension solution;
(3) black suspension solution is poured in the hydrothermal reaction kettle, reacted 12 hours down at 120 ℃;
(4) after hydro-thermal reaction finishes, reactant is carried out centrifugation, obtain solid product; Solid product is used distilled water and washing with alcohol successively, obtain olive shape tellurium nanocrystals particle after the drying.
Embodiment 3
Preparation tellurium nanometer stub, concrete steps are:
(1) positive telluric acid is dissolved in the water, forming concentration is 4 * 10
-2The telluric aqueous acid of mol/L;
(2) hydrazine hydrate of 40 mmoles is joined in 40 milliliters the telluric aqueous acid, form black suspension solution;
(3) black suspension solution is poured in the hydrothermal reaction kettle, reacted 18 hours down at 110 ℃;
(4) after hydro-thermal reaction finishes, reactant is carried out centrifugation, obtain solid product; Solid product is used distilled water and washing with alcohol successively, obtain tellurium nanometer stub after the drying.
Embodiment 4
Preparation tellurium nanometer stub, concrete steps are:
(1) positive telluric acid is dissolved in the water, forming concentration is 3 * 10
-2The telluric aqueous acid of mol/L;
(2) hydrazine hydrate of 50 mmoles is joined in 50 milliliters the telluric aqueous acid, form black suspension solution;
(3) black suspension solution is poured in the hydrothermal reaction kettle, reacted 24 hours down at 120 ℃;
(4) after hydro-thermal reaction finishes, reactant is carried out centrifugation, obtain solid product; Solid product is used distilled water and washing with alcohol successively, obtain tellurium nanometer stub after the drying.
Embodiment 5
Preparation tellurium nanometer stub, concrete steps are:
(1) positive telluric acid is dissolved in the water, forming concentration is 3.5 * 10
-2The telluric aqueous acid of mol/L;
(2) hydrazine hydrate of 50 mmoles is joined in 40 milliliters the telluric aqueous acid, form black suspension solution;
(3) black suspension solution is poured in the hydrothermal reaction kettle, reacted 18 hours down at 100 ℃;
(4) after hydro-thermal reaction finishes, reactant is carried out centrifugation, obtain solid product; Solid product is used distilled water and washing with alcohol successively, obtain tellurium nanometer stub after the drying.
Embodiment 6
The long rod of preparation tellurium nanometer, concrete steps are:
(1) positive telluric acid is dissolved in the water, forming concentration is 2 * 10
-2The telluric aqueous acid of mol/L;
(2) hydrazine hydrate of 60 mmoles is joined in 60 milliliters the telluric aqueous acid, form black suspension solution;
(3) black suspension solution is poured in the hydrothermal reaction kettle, reacted 15 hours down at 110 ℃;
(4) after hydro-thermal reaction finishes, reactant is carried out centrifugation, obtain solid product; Solid product is used distilled water and washing with alcohol successively, obtain the long rod of the about 10 microns tellurium nanometer of length after the drying.
Embodiment 7
The long rod of preparation tellurium nanometer, concrete steps are:
(1) positive telluric acid is dissolved in the water, forming concentration is 1 * 10
-2The telluric aqueous acid of mol/L;
(2) hydrazine hydrate of 80 mmoles is joined in 50 milliliters the telluric aqueous acid, form black suspension solution;
(3) black suspension solution is poured in the hydrothermal reaction kettle, reacted 12 hours down at 100 ℃;
(4) after hydro-thermal reaction finishes, reactant is carried out centrifugation, obtain solid product; Solid product is used distilled water and washing with alcohol successively, obtain the long rod of the about 25 microns tellurium nanometer of length after the drying.
Claims (1)
1. preparing tellurium nanocrystals is characterized in that these method concrete steps are as follows:
(1) positive telluric acid is dissolved in the water, the pattern configuration telluric aqueous acid required according to the tellurium nanocrystals of preparation, specifically:
Prepare the tellurium nanocrystals particle as need, then Pei Zhi telluric aqueous acid concentration is M
1, 4 * 10
-2Mol/L＜M
1≤ 6 * 10
-2Mol/L;
Prepare the tellurium nanometer stub that length is 100～200 nanometers as need, then Pei Zhi telluric aqueous acid concentration is M
2, 3 * 10
-2Mol/L≤M
2≤ 4 * 10
-2Mol/L;
Prepare the tellurium nanometer long rod of length greater than 200 nanometers as need, then Pei Zhi telluric aqueous acid concentration is M
3, 1 * 10
-2Mol/L≤M
3＜3 * 10
-2Mol/L;
(2) reductive agent one hydrazine hydrate is joined in the telluric aqueous acid, form black suspension solution; The amount that every milliliter of telluric aqueous acid adds a hydrazine hydrate is 1～2 mmole;
(3) black suspension solution is poured into carried out hydro-thermal reaction in the hydrothermal reaction kettle, temperature of reaction is 100～120 ℃, and the reaction times is 12～24 hours;
(4) after hydro-thermal reaction finishes, reactant is carried out centrifugation, obtain solid product; Solid product is used distilled water and washing with alcohol successively, obtain the black solid powder after the drying, be tellurium nanocrystals.
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|---|---|---|---|
| CN2010102622025A CN101920940B (en) | 2010-08-20 | 2010-08-20 | Method for preparing tellurium nanocrystals |
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| CN2010102622025A CN101920940B (en) | 2010-08-20 | 2010-08-20 | Method for preparing tellurium nanocrystals |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102583267A (en) * | 2012-02-21 | 2012-07-18 | 合肥工业大学 | Method for preparing electron spin resonance standard substance by using hydrothermal method |
| CN102583269A (en) * | 2012-03-30 | 2012-07-18 | 哈尔滨工业大学 | Needle-shaped monocrystal tellurium and preparation method thereof |
| US20130252406A1 (en) * | 2012-03-23 | 2013-09-26 | Evident Technologies, Inc. | Techniques for drying and annealing thermoelectric powders |
| CN103373713A (en) * | 2012-04-25 | 2013-10-30 | 中国科学院合肥物质科学研究院 | Tellurium nano-particles and preparation method for same |
| RU2629679C1 (en) * | 2016-11-29 | 2017-08-31 | Акционерное общество "Производственное объединение "Электрохимический завод" | Method for elemental tellurium production |
| CN110862089A (en) * | 2019-12-09 | 2020-03-06 | 徐少晨 | Preparation method of mesoporous hollow silicon spheres |
| CN111186822A (en) * | 2018-11-15 | 2020-05-22 | 南京理工大学 | Preparation method of tellurium nanoparticles |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1661138A (en) * | 2004-12-17 | 2005-08-31 | 南京大学 | Method for fast preparing single crystal tellurium in one dimension Nano structure from powder of fellurium |
| CN1721321A (en) * | 2005-05-13 | 2006-01-18 | 中国科学院上海硅酸盐研究所 | A kind of method for preparing the simple substance nano powder with the reductive agent reduced oxide |
-
2010
- 2010-08-20 CN CN2010102622025A patent/CN101920940B/en not_active Expired - Fee Related
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1661138A (en) * | 2004-12-17 | 2005-08-31 | 南京大学 | Method for fast preparing single crystal tellurium in one dimension Nano structure from powder of fellurium |
| CN1721321A (en) * | 2005-05-13 | 2006-01-18 | 中国科学院上海硅酸盐研究所 | A kind of method for preparing the simple substance nano powder with the reductive agent reduced oxide |
Non-Patent Citations (1)
| Title |
|---|
| 《Advanced Materials》 20020219 Brian Mayers, et al. Formation of tellurium nanotubes through concentration depletion at the surfaces of seeds 第280页左栏第4行至第18行 1 第14卷, 第4期 2 * |
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102583267A (en) * | 2012-02-21 | 2012-07-18 | 合肥工业大学 | Method for preparing electron spin resonance standard substance by using hydrothermal method |
| US20130252406A1 (en) * | 2012-03-23 | 2013-09-26 | Evident Technologies, Inc. | Techniques for drying and annealing thermoelectric powders |
| CN102583269A (en) * | 2012-03-30 | 2012-07-18 | 哈尔滨工业大学 | Needle-shaped monocrystal tellurium and preparation method thereof |
| CN103373713A (en) * | 2012-04-25 | 2013-10-30 | 中国科学院合肥物质科学研究院 | Tellurium nano-particles and preparation method for same |
| RU2629679C1 (en) * | 2016-11-29 | 2017-08-31 | Акционерное общество "Производственное объединение "Электрохимический завод" | Method for elemental tellurium production |
| CN111186822A (en) * | 2018-11-15 | 2020-05-22 | 南京理工大学 | Preparation method of tellurium nanoparticles |
| CN111186822B (en) * | 2018-11-15 | 2022-12-02 | 南京理工大学 | Preparation method of tellurium nanoparticles |
| CN110862089A (en) * | 2019-12-09 | 2020-03-06 | 徐少晨 | Preparation method of mesoporous hollow silicon spheres |
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|---|---|
| CN101920940B (en) | 2012-03-28 |
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