CN100560479C - A kind of Bi 2Te 3The preparation method of nano flake - Google Patents
A kind of Bi 2Te 3The preparation method of nano flake Download PDFInfo
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- CN100560479C CN100560479C CNB2008100625727A CN200810062572A CN100560479C CN 100560479 C CN100560479 C CN 100560479C CN B2008100625727 A CNB2008100625727 A CN B2008100625727A CN 200810062572 A CN200810062572 A CN 200810062572A CN 100560479 C CN100560479 C CN 100560479C
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Abstract
The invention discloses a kind of preparation Bi
2Te
3The method of nano flake.This method adopts low temperature wet to learn synthesis technique.To contain the compound of Bi and Te simple substance according to the determined mixed of final product chemical ingredients in deionized water.Add the reductive agent of capacity and suitable complexing agent, under 95-110 ℃ of temperature, rely on boiling to stir, reaction 24-48h, centrifugation, washing, oven dry get final product.Its pattern is the Polygons nano flake.This method technology is simple, need not to add alkaline conditioner, and the product form that obtains is unified, and its pattern is the Polygons nano flake, and the product purity height is expected to improve Bi
2Te
3The thermoelectricity capability of base thermoelectricity material, and can be widely used in fields such as physics, chemistry, microelectronics, material.
Description
Technical field
The present invention relates to Bi
2Te
3The preparation method of nanometer powder belongs to the semi-conductor thermoelectric material technical field.
Background technology
Thermoelectric material is also referred to as thermoelectric material, is a kind of functional materials that can realize direct mutual conversion between heat energy and the electric energy.The device of making of thermoelectric material has that volume is little, noiselessness, pollution-free, movement-less part, outstanding advantage such as non-maintaining, has important application prospects aspect thermoelectric (al) cooling and the thermo-electric generation.Study, develop and promote thermoelectric cooling and thermo-electric generation technology energetically, all have important value for China and even global energy utilization, Economic development and environment protection etc.
Bi
2Te
3Compound and solid solution alloy thereof are to study the earliest, also are to develop one of the most sophisticated thermoelectric material at present, are applicable near the room temperature that the ZT value (thermoelectric figure of merit) that characterizes thermoelectricity capability is 0.8～1, and present most of cooling elements all adopt this class material.The nanometer that studies show that material can improve the phon scattering effect, and then improves the thermoelectricity capability of material.
Solvent thermal or hydro-thermal are synthesized Bi
2Te
3Be preparation Bi
2Te
3The effective way of nano particle.This method technology is simple, product purity is high.But all added alkaline conditioner in the synthesis technique of having reported, and have document (X.B.Zhao, T.Sun, T.J.Zhu and J.P.Tu.J.Mater.Chem., 2005,15,1621-1625) indicate: do not add alkaline conditioner, can't obtain Bi
2Te
3Nanometer powder.And the nanometer powder form that generally obtains is varied, sees document X.B.Zhao, X.H.Ji, and Y.H.Zhang.Appl.Phys.A 80, and 1567-1571 (2005) reports (Figure 2).
Summary of the invention
The purpose of this invention is to provide and a kind ofly need not to add alkaline conditioner, and the unified preparation Bi of product form
2Te
3The method of nano flake.
Bi of the present invention
2Te
3The preparation method of nano flake, employing be the synthetic method that low temperature wet is learned, its step is as follows:
1) will contain the compound of Bi element and Te simple substance according to final product Bi
2Te
3The determined mixed of chemical ingredients in deionized water, the 600-1000 that the quality of deionized water is equivalent to Te simple substance quality doubly fully mixes;
2) above-mentioned mixed solution is placed in the reaction vessel, add the complexing agent of the 40-60% that is equivalent to Te simple substance quality and the reductive agent of capacity;
3) reaction vessel is warming up to 95-110 ℃ a certain temperature value, makes the aqueous solution keep boiling, reaction 24-48h postcooling is to room temperature;
4) collect the interior solid product of reaction vessel, centrifugation, washing, oven dry obtain Bi
2Te
3Nano flake.
The above-mentioned compound that contains the Bi element is muriate, oxide compound, vitriol, nitrate or carbonate.
Above-mentioned complexing agent is EDTA disodium salt, citric acid, Trisodium Citrate or ethylenediamine tetraacetic acid (EDTA).Said reductive agent is NaBH
4, KBH
4, alkali-metal hydroborate or Na, K basic metal.
The invention provides Bi
2Te
3Preparation of sections method technology is simple, need not to add alkaline conditioner, and the product form that obtains is unified, and its pattern is the Polygons nano flake, and the product purity height is expected to improve Bi
2Te
3The thermoelectricity capability of base thermoelectricity material, and can be widely used in fields such as physics, chemistry, microelectronics, material.
Description of drawings
Fig. 1 is that the 48h low temperature wet is learned synthetic Bi
2Te
3The scanning electron microscope high magnification photo of nano flake;
Fig. 2 is that the 48h low temperature wet is learned synthetic Bi
2Te
3The scanning electron microscope low range photo of nano flake;
Fig. 3 is that the 24h low temperature wet is learned synthetic Bi
2Te
3The scanning electron microscope high magnification photo of nano flake.
Embodiment
Below in conjunction with embodiment the present invention is done and to describe in further detail.
Embodiment 1
In the three neck round-bottomed flasks of 500ml, add the 150g deionized water, add Te powder 0.19g (about 1.5mmol, purity is 99.999%, crosses 300 mesh sieves) and BiCl again
30.21g (about 1mmol, analytical pure) fully mixes, and adds NaBH again
40.4g, EDTA disodium salt 0.1g; Three neck round-bottomed flask temperature are transferred to 100 ℃.Intermediary interface place at flask connects a prolong, and the water vapour of condensing reflux evaporation guarantees that strength of solution remains unchanged in the reaction.Constantly attemperation makes solution be in the ebullient state, reaches the purpose of stirring with this.React after 48 hours, the water source of powered-down and prolong is cooled to room temperature., washing centrifugal, collect solid product with deionized water, dehydrated alcohol.Get Bi after 60 ℃ of dryings
2Te
3Powder.
Adopt the thing phase of Rigaku-D/MAX-2550PC type X ray polycrystalline diffractometer assay products, the result is monophasic Bi
2Te
3Adopt SIRION-FEI type field emission scanning electron microscope to observe its microscopic pattern.Be mainly laminarly, its thickness is about tens nanometers (seeing Fig. 1, Fig. 2).
Embodiment 2
In the three neck round-bottomed flasks of 500ml, add the 150g deionized water, add Te powder 0.19g (about 1.5mmol, purity is 99.999%, crosses 300 mesh sieves) and BiCl again
30.21g (about 1mmol, analytical pure) fully mixes, and adds NaBH again
40.4g, EDTA disodium salt 0.1g; Three neck round-bottomed flask temperature are transferred to 100 ℃.Intermediary interface place at flask connects a prolong, and the water vapour of condensing reflux evaporation guarantees that strength of solution remains unchanged in the reaction.Constantly attemperation makes solution be in the ebullient state, reaches the purpose of stirring with this.React after 24 hours, the water source of powered-down and prolong is cooled to room temperature., washing centrifugal, collect solid product with deionized water, dehydrated alcohol.Get Bi after 60 ℃ of dryings
2Te
3Powder.
Adopt the thing phase of Rigaku-D/MAX-2550PC type X ray polycrystalline diffractometer assay products, the result is monophasic Bi
2Te
3Adopt SIRION-FEI type field emission scanning electron microscope to observe its microscopic pattern.Be mainly laminarly, its thickness is about tens nanometer (see figure 3)s.
Embodiment 3
In the three neck round-bottomed flasks of 500ml, add the 150g deionized water, add Te powder 0.19g (about 1.5mmol, purity is 99.999%, crosses 300 mesh sieves) and Bi (NO again
3)
35H
2O0.49g (about 1mmol, analytical pure) fully mixes, and adds KBH again
40.5g, EDTA disodium salt 0.1g; Three neck round-bottomed flask temperature are transferred to 100 ℃.Intermediary interface place at flask connects a prolong, and the water vapour of condensing reflux evaporation guarantees that strength of solution remains unchanged in the reaction.Constantly attemperation makes solution be in the ebullient state, reaches the purpose of stirring with this.React after 36 hours, the water source of powered-down and prolong is cooled to room temperature., washing centrifugal, collect solid product with deionized water, dehydrated alcohol.Get Bi after 60 ℃ of dryings
2Te
3Powder.Adopt SIRION-FEI type field emission scanning electron microscope to observe its microscopic pattern, be mainly laminarly, its thickness is about tens nanometers.
Embodiment 4
In the three neck round-bottomed flasks of 500ml, add the 150g deionized water, add Te powder 0.19g (about 1.5mmol, purity is 99.999%, crosses 300 mesh sieves) and Bi again
2(CO
3)
30.3g (about 0.5mmol, analytical pure) fully mixes, and adds NaBH again
40.4g, Trisodium Citrate 0.2g; Three neck round-bottomed flask temperature are transferred to 100 ℃.Intermediary interface place at flask connects a prolong, and the water vapour of condensing reflux evaporation guarantees that strength of solution remains unchanged in the reaction.Constantly attemperation makes solution be in the ebullient state, reaches the purpose of stirring with this.React after 24 hours, the water source of powered-down and prolong is cooled to room temperature., washing centrifugal, collect solid product with deionized water, dehydrated alcohol.Get Bi after 60 ℃ of dryings
2Te
3Powder.Adopt SIRION-FEI type field emission scanning electron microscope to observe its microscopic pattern, be mainly laminarly, its thickness is about tens nanometers.
Claims (4)
1. Bi
2Te
3The preparation method of nano flake, its step is as follows:
1) will contain the compound of Bi element and Te simple substance according to final product Bi
2Te
3The determined mixed of chemical ingredients in deionized water, the 600-1000 that the quality of deionized water is equivalent to Te simple substance quality doubly fully mixes;
2) above-mentioned mixed solution is placed in the reaction vessel, add the complexing agent of the 40-60% that is equivalent to Te simple substance quality and the reductive agent of capacity;
3) reaction vessel is warming up to 95-110 ℃ a certain temperature value, makes the aqueous solution keep boiling, reaction 24-48h postcooling is to room temperature;
4) collect the interior solid product of reaction vessel, centrifugation, washing, oven dry obtain Bi
2Te
3Nano flake.
2. Bi according to claim 1
2Te
3The preparation method of nano flake, the compound that it is characterized in that said Bi element is muriate, oxide compound, vitriol, nitrate or carbonate.
3. Bi according to claim 1
2Te
3The preparation method of nano flake is characterized in that said complexing agent is EDTA disodium salt, citric acid, Trisodium Citrate or ethylenediamine tetraacetic acid (EDTA).
4. Bi according to claim 1
2Te
3The preparation method of nano flake is characterized in that said reductive agent is NaBH
4, KBH
4Or Na, K basic metal.
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Families Citing this family (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101513994B (en) * | 2009-03-10 | 2011-10-05 | 中国科学院上海硅酸盐研究所 | Bismuth base hydrogen storage material and preparation method thereof |
| CN103058152A (en) * | 2013-01-16 | 2013-04-24 | 吉林大学 | Non-bismuth-telluride-doped magnetic material and preparation method thereof |
| CN109569475A (en) * | 2017-09-28 | 2019-04-05 | 中国电力科学研究院 | A kind of thermoelectric material preparation facilities and method |
| CN108584887A (en) * | 2018-03-07 | 2018-09-28 | 南京航空航天大学 | A kind of Bi with 3-D nano, structure2Te3Material and its preparation method and application |
| CN112316935B (en) * | 2020-11-25 | 2022-05-24 | 正太新材料科技有限责任公司 | Preparation method for degrading and separating flaky Bi-based catalytic pigment |
| CN112723322A (en) * | 2021-01-29 | 2021-04-30 | 河南科技大学 | Method for preparing layered bismuth telluride nanoparticles by hydrothermal method |
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Non-Patent Citations (4)
| Title |
|---|
| A novel approach to Bi2Te3 nanorods by controlling orientedattachment. Yuan Deng et al.Chemical Physics Letters,Vol.383 . 2004 |
| A novel approach to Bi2Te3 nanorods by controlling orientedattachment. Yuan Deng et al.Chemical Physics Letters,Vol.383 . 2004 * |
| 纳米结构Bi2Te3化合物的低温湿化学合成. 孙霆等.化学学报，第63卷第16期. 2005 |
| 纳米结构Bi2Te3化合物的低温湿化学合成. 孙霆等.化学学报，第63卷第16期. 2005 * |
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