CN103058151A - Hiberarchy bismuth telluride nanocrystal and preparation method thereof - Google Patents
Hiberarchy bismuth telluride nanocrystal and preparation method thereof Download PDFInfo
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- CN103058151A CN103058151A CN2013100163485A CN201310016348A CN103058151A CN 103058151 A CN103058151 A CN 103058151A CN 2013100163485 A CN2013100163485 A CN 2013100163485A CN 201310016348 A CN201310016348 A CN 201310016348A CN 103058151 A CN103058151 A CN 103058151A
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Abstract
The invention relates to a hiberarchy bismuth telluride nanocrystal and a preparation method thereof, belonging to the technical field of nanometer materials and synthesis methods thereof. The preparation method comprises the following steps of putting bismuth acetate, oleic acid and octadecene into a container and stirring with magnetic force, heating up under the protection of nitrogen till completely dissolving bismuth acetate, then cooling down to room temperature, adding trioctylphosphine solution of tellurium prepared in advance into the container at room temperature, reacting at 140-240 DEG C, and keeping the temperature for 0.5-6 hours. The hiberarchy bismuth telluride nanocrystal is prepared by a sol-gel method, and the grain size and appearance of the bismuth telluride nanocrystal can be controlled by changing the reaction time and temperature.
Description
Technical field
The invention belongs to the technical field of nano material and synthetic method thereof, particularly nanocrystalline the and method of a kind of (hierarchical) for preparing hierarchy.
Background technology
Because the burning of coal and the discharging of vehicle exhaust cause gradually global warming and produce a lot of used heat.The overdevelopment electric material then is the effective way that addresses this problem, and converts the electric energy useful to the mankind to because thermoelectric material can utilize extraneous used heat.Tellurobismuthite (Bi
2Te
3) owing to having high quality factor (ZT) under the room temperature, therefore in traditional technology, usually be widely studied as thermoelectric material potential under the room temperature.And nano material can effectively reduce lattice thermal conductivity for the body material, thereby improves the thermoelectricity capability of nano material.Recently, Bi
2Te
3One of be suggested as the simplest three-dimensional topology isolator, the body electronic state of this polymorphic material is that its surface of isolator of energy gap is arranged then is metallic state without energy gap.With respect to macroscopical block materials, topological isolator nano material has large specific surface area, the contribution of energy establishment figure current carrier, thus highlight topological surperficial state property matter.Therefore, people are seeking a kind of more effective means always and are realizing Bi
2Te
3Preparation.
Existing Bi
2Te
3All be to form by the solid state powder sintering under the comparatively high temps, or utilize ball mill grinding to make corresponding pressed powder.And great majority are based on the Bi of body material
2Te
3Preparation.So far, utilize the colloid chemistry method to prepare the Bi of hierarchy
2Te
3The nanocrystalline report that yet there are no.
Summary of the invention
The technical problem to be solved in the present invention is, provides a kind of Tellurobismuthite that utilizes sol-gel method to prepare hierarchy nanocrystalline method, the simple easy handling of the method, and realize that size, pattern are controlled.
The technical characterictic of product of the present invention is as described below:
A kind of Tellurobismuthite of hierarchy is nanocrystalline, and molecular formula is Bi
2Te
3The similar nanometer sheet of pattern be crossed as flower-shaped after, link to each other to consist of the caterpillar shape; Mean diameter is 230 ~ 565nm.
Preparation hierarchy Bi
2Te
3Nanocrystalline technical scheme is:
The preparation method that a kind of Tellurobismuthite of hierarchy is nanocrystalline has following process,
(1) the tri octyl phosphine solution of preparation tellurium: tellurium powder and tri octyl phosphine are mixed, naturally be down to room temperature after keeping 2 ~ 4 hours being warming up to 200 ~ 250 ℃ under the protection of nitrogen, the tri octyl phosphine solution storage of tellurium that obtains concentration and be 0.2mol/L is for subsequent use;
(2) hierarchy Bi
2Te
3Nanocrystalline preparation: with bismuth acetate, oleic acid and octadecylene are packed into and are carried out magnetic agitation in the container, be warming up to bismuth acetate and dissolve fully under the protection of nitrogen; Be down to gradually afterwards room temperature, the tri octyl phosphine solution of tellurium is joined in the container, under 140 ~ 240 ℃, react and be incubated 0.5 ~ 6 hour; Obtain the Tellurobismuthite powder through the centrifugal sample of washing; Bismuth acetate in molar ratio wherein: tellurium=2: 3, by volume oleic acid: octadecylene=1: 6, the consumption of oleic acid add 5mL oleic acid by every mmol bismuth acetate and calculate.
The described centrifugal sample of washing carries out according to a conventional method.
The invention has the beneficial effects as follows and prepare Bi
2Te
3Nanocrystalline; And can by changing temperature of reaction and soaking time, realize size, the controlled nanocrystalline preparation of Tellurobismuthite of pattern.
Description of drawings
Fig. 1 is the Bi of embodiment 2 preparations
2Te
3The X-ray diffraction spectrum of sample.
Fig. 2 is that embodiment 2 is at 140 ℃ of Bi that prepare after keeping 2 hours
2Te
3The stereoscan photograph of sample.
Fig. 3 is that embodiment 3 is at 160 ℃ of Bi that prepare after keeping 2 hours
2Te
3The stereoscan photograph of sample.
Fig. 4 is that embodiment 4 is at 180 ℃ of Bi that prepare after keeping 2 hours
2Te
3The stereoscan photograph of sample.
Fig. 5 is that embodiment 5 is at 200 ℃ of Bi that prepare after keeping 2 hours
2Te
3The stereoscan photograph of sample.
Fig. 6 is that embodiment 6 is at 220 ℃ of Bi that prepare after keeping 2 hours
2Te
3The stereoscan photograph of sample.
Fig. 7 is that embodiment 7 is at 240 ℃ of Bi that prepare after keeping 2 hours
2Te
3The stereoscan photograph of sample.
Fig. 8 is that embodiment 8 is at 200 ℃ of Bi that prepare after keeping 30 minutes
2Te
3The stereoscan photograph of sample.
Fig. 9 is that embodiment 9 is at 200 ℃ of Bi that prepare after keeping 1 hour
2Te
3The stereoscan photograph of sample.
Figure 10 is that embodiment 9 is at 200 ℃ of Bi that prepare after keeping 1 hour
2Te
3The high-resolution-ration transmission electric-lens photo of sample.
Figure 11 is that embodiment 10 is at 200 ℃ of Bi that prepare after keeping 4 hours
2Te
3The stereoscan photograph of sample.
Figure 12 is that embodiment 11 is at 200 ℃ of Bi that prepare after keeping 6 hours
2Te
3The stereoscan photograph of sample.
Embodiment
Now more specifically describe the present invention in conjunction with the following example, if no special instructions, agents useful for same is commercially available obtainable product, does not add further purification and uses.
The preparation of the tri octyl phosphine solution of embodiment 1 tellurium
Compound concentration is the tri octyl phosphine solution of the tellurium of 0.2mol/L, and concrete operations technique is as follows: tellurium powder and tri octyl phosphine are mixed in the 50mL round bottom three-necked bottle, be warming up under the protection of nitrogen 200 ℃ keep 4 hours after naturally near room temperature, and storage is with for subsequent use.
Also can be warming up under the protection of nitrogen 250 ℃ keep 2 hours after naturally near room temperature, prepare and obtain the tri octyl phosphine solution that concentration is the tellurium of 0.2mol/L.
Embodiment 2 is 140 ℃ of hierarchy Bi that prepare after keeping 2 hours in temperature of reaction
2Te
3Nanocrystalline
At first with the 0.2mmol bismuth acetate, 1mL oleic acid and 6mL octadecylene are packed in the 50mL round bottom three-necked bottle and are accompanied by strong magnetic agitation, progressively be warming up to bismuth acetate and dissolve fully under the protection of nitrogen.Be down to gradually subsequently room temperature.The tri octyl phosphine solution 1.5mL of the 0.2mol/L tellurium that at room temperature will prepare in advance joins in the three-necked bottle, then rises to 140 ℃ and kept 2 hours.Fig. 1 is the X-ray diffractogram of the sample that makes, is rhombohedral Bi
2Te
3As shown in Figure 2, can see hierarchy Bi from the stereoscan photograph of prepared sample
2Te
3Nanocrystalline diameter is 230nm.
At first with the 0.2mmol bismuth acetate, 1mL oleic acid and 6mL octadecylene are packed in the 50mL round bottom three-necked bottle and are accompanied by strong magnetic agitation, progressively be warming up to bismuth acetate and dissolve fully under the protection of nitrogen.Be down to gradually subsequently room temperature.The tri octyl phosphine solution 1.5mL of the 0.2mol/L tellurium that at room temperature will prepare in advance joins in the three-necked bottle, then rises to 160 ℃ and kept 2 hours.As shown in Figure 3, can see hierarchy Bi from the stereoscan photograph of prepared sample
2Te
3Nanocrystalline diameter is 345nm.
Embodiment 4 is 180 ℃ of hierarchy Bi that prepare after keeping 2 hours in temperature of reaction
2Te
3Nanocrystalline
At first with the 0.2mmol bismuth acetate, 1mL oleic acid and 6mL octadecylene are packed in the 50mL round bottom three-necked bottle and are accompanied by strong magnetic agitation, progressively be warming up to bismuth acetate and dissolve fully under the protection of nitrogen.Be down to gradually subsequently room temperature.The tri octyl phosphine solution 1.5mL of the 0.2mol/L tellurium that at room temperature will prepare in advance joins in the three-necked bottle, then rises to 180 ℃ and kept 2 hours.As shown in Figure 4, can see hierarchy Bi from the stereoscan photograph of prepared sample
2Te
3Nanocrystalline diameter is 450nm.
Embodiment 5 is 200 ℃ of hierarchy Bi that prepare after keeping 2 hours in temperature of reaction
2Te
3Nanocrystalline
At first with the 0.2mmol bismuth acetate, 1mL oleic acid and 6mL octadecylene are packed in the 50mL round bottom three-necked bottle and are accompanied by strong magnetic agitation, progressively be warming up to bismuth acetate and dissolve fully under the protection of nitrogen.Be down to gradually subsequently room temperature.The tri octyl phosphine solution 1.5mL of the 0.2mol/L tellurium that at room temperature will prepare in advance joins in the three-necked bottle, then rises to 200 ℃ and kept 2 hours.As shown in Figure 5, can see hierarchy Bi from the stereoscan photograph of prepared sample
2Te
3Nanocrystalline diameter is 470nm.
Embodiment 6 is 220 ℃ of hierarchy Bi that prepare after keeping 2 hours in temperature of reaction
2Te
3Nanocrystalline
At first with the 0.2mmol bismuth acetate, 1mL oleic acid and 6mL octadecylene are packed in the 50mL round bottom three-necked bottle and are accompanied by strong magnetic agitation, progressively be warming up to bismuth acetate and dissolve fully under the protection of nitrogen.Be down to gradually subsequently room temperature.The tri octyl phosphine solution 1.5mL of the 0.2mol/L tellurium that at room temperature will prepare in advance joins in the three-necked bottle, then rises to 220 ℃ and kept 2 hours.As shown in Figure 6, can see hierarchy Bi from the stereoscan photograph of prepared sample
2Te
3Nanocrystalline diameter is 520nm.
Embodiment 7 is 240 ℃ of hierarchy Bi that prepare after keeping 2 hours in temperature of reaction
2Te
3Nanocrystalline
At first with the 0.2mmol bismuth acetate, 1mL oleic acid and 6mL octadecylene are packed in the 50mL round bottom three-necked bottle and are accompanied by strong magnetic agitation, progressively be warming up to bismuth acetate and dissolve fully under the protection of nitrogen.Be down to gradually subsequently room temperature.The tri octyl phosphine solution 1.5mL of the 0.2mol/L tellurium that at room temperature will prepare in advance joins in the three-necked bottle, then rises to 240 ℃ and kept 2 hours.As shown in Figure 7, can see hierarchy Bi from the stereoscan photograph of prepared sample
2Te
3Nanocrystalline diameter is 565nm.
Embodiment 8 is 200 ℃ of hierarchy Bi that prepare after keeping 30 minutes in temperature of reaction
2Te
3Nanocrystalline
At first with the 0.2mmol bismuth acetate, 1mL oleic acid and 6mL octadecylene are packed in the 50mL round bottom three-necked bottle and are accompanied by strong magnetic agitation, progressively be warming up to bismuth acetate and dissolve fully under the protection of nitrogen.Be down to gradually subsequently room temperature.The tri octyl phosphine solution 1.5mL of the 0.2mol/L tellurium that at room temperature will prepare in advance joins in the three-necked bottle, then rises to 200 ℃ and kept 30 minutes.As shown in Figure 8, can see hierarchy Bi from the stereoscan photograph of prepared sample
2Te
3Nanocrystalline diameter is 320nm.
Embodiment 9 is 200 ℃ of hierarchy Bi that prepare after keeping 1 hour in temperature of reaction
2Te
3Nanocrystalline
At first with the 0.2mmol bismuth acetate, 1mL oleic acid and 6mL octadecylene are packed in the 50mL round bottom three-necked bottle and are accompanied by strong magnetic agitation, progressively be warming up to bismuth acetate and dissolve fully under the protection of nitrogen.Be down to gradually subsequently room temperature.The tri octyl phosphine solution 1.5mL of the 0.2mol/L tellurium that at room temperature will prepare in advance joins in the three-necked bottle, then rises to 200 ℃ and kept 1 hour.As shown in Figure 9, can see hierarchy Bi from the stereoscan photograph of prepared sample
2Te
3Nanocrystalline diameter is 430nm.The high resolution transmission electron microscopy of the sample from Figure 10 can see, fringe spacing is
Corresponding to rhombohedral (015) spacing.
At first with the 0.2mmol bismuth acetate, 1mL oleic acid and 6mL octadecylene are packed in the 50mL round bottom three-necked bottle and are accompanied by strong magnetic agitation, progressively be warming up to bismuth acetate and dissolve fully under the protection of nitrogen.Be down to gradually subsequently room temperature.The tri octyl phosphine solution 1.5mL of the 0.2mol/L tellurium that at room temperature will prepare in advance joins in the three-necked bottle, then rises to 200 ℃ and kept 4 hours.As shown in figure 11, can see hierarchy Bi from the stereoscan photograph of prepared sample
2Te
3Nanocrystalline diameter is 535nm.
Embodiment 11 is 200 ℃ of hierarchy Bi that prepare after keeping 6 hours in temperature of reaction
2Te
3Nanocrystalline
At first with the 0.2mmol bismuth acetate, 1mL oleic acid and 6mL octadecylene are packed in the 50mL round bottom three-necked bottle and are accompanied by strong magnetic agitation, progressively be warming up to bismuth acetate and dissolve fully under the protection of nitrogen.Be down to gradually subsequently room temperature.The tri octyl phosphine solution 1.5mL of the 0.2mol/L tellurium that at room temperature will prepare in advance joins in the three-necked bottle, then rises to 200 ℃ and kept 6 hours.As shown in figure 12, can see hierarchy Bi from the stereoscan photograph of prepared sample
2Te
3Nanocrystalline diameter is about 550nm.
Claims (2)
1. the Tellurobismuthite of a hierarchy is nanocrystalline, and molecular formula is Bi
2Te
3Pattern be nanometer sheet be crossed as flower-shaped after, link to each other to consist of the caterpillar shape; Mean diameter is 230 ~ 565nm.
2. the nanocrystalline preparation method of the Tellurobismuthite of the hierarchy of a claim 1 has following process,
(1) the tri octyl phosphine solution of preparation tellurium: tellurium powder and tri octyl phosphine are mixed, naturally be down to room temperature after keeping 2 ~ 4 hours being warming up to 200 ~ 250 ℃ under the protection of nitrogen, the tri octyl phosphine solution storage of tellurium that obtains concentration and be 0.2mol/L is for subsequent use;
(2) hierarchy Bi
2Te
3Nanocrystalline preparation: with bismuth acetate, oleic acid and octadecylene are packed into and are carried out magnetic agitation in the container, be warming up to bismuth acetate and dissolve fully under the protection of nitrogen; Be down to afterwards room temperature, the tri octyl phosphine solution of tellurium is joined in the container, under 140 ~ 240 ℃, react and be incubated 0.5 ~ 6 hour; Obtain the Tellurobismuthite powder through the centrifugal sample of washing; Bismuth acetate in molar ratio wherein: tellurium=2: 3, by volume oleic acid: octadecylene=1: 6, the consumption of oleic acid add 5mL oleic acid by every mmol bismuth acetate and calculate.
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Cited By (2)
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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 |
CN113149076A (en) * | 2021-05-27 | 2021-07-23 | 吉林大学 | Preparation method of phosphorus-selenium co-doped niobium disulfide nano material |
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CN1384048A (en) * | 2002-06-21 | 2002-12-11 | 清华大学 | Nano level metal telluride preparing process |
US6872330B2 (en) * | 2002-05-30 | 2005-03-29 | The Regents Of The University Of California | Chemical manufacture of nanostructured materials |
CN101513994A (en) * | 2009-03-10 | 2009-08-26 | 中国科学院上海硅酸盐研究所 | Bismuth base hydrogen storage material and preparation method thereof |
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US6872330B2 (en) * | 2002-05-30 | 2005-03-29 | The Regents Of The University Of California | Chemical manufacture of nanostructured materials |
CN1384048A (en) * | 2002-06-21 | 2002-12-11 | 清华大学 | Nano level metal telluride preparing process |
CN101513994A (en) * | 2009-03-10 | 2009-08-26 | 中国科学院上海硅酸盐研究所 | Bismuth base hydrogen storage material and preparation method thereof |
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JAE SUNG SON等: "n-Type Nanostructured Thermoelectric Materials Prepared from Chemically Synthesized Ultrathin Bi2Te3 Nanoplates", 《NANO LETTERS》 * |
JIPENG FU等: "Bi2Te3 nanoplates and nanoflowers: Synthesized by hydrothermal process and their enhanced thermoelectric properties", 《CRYSTENGCOMM》 * |
LIANGLIANG CHEN等: "Facile synthesis of ultra-small Bi2Te3 nanoparticles, nanorods and nanoplates and their morphology-dependent Raman spectroscopy", 《MATERIALS LETTERS》 * |
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Cited By (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
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 |
CN113149076A (en) * | 2021-05-27 | 2021-07-23 | 吉林大学 | Preparation method of phosphorus-selenium co-doped niobium disulfide nano material |
CN113149076B (en) * | 2021-05-27 | 2022-07-01 | 吉林大学 | Preparation method of phosphorus-selenium co-doped niobium disulfide nano material |
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