CN109950138B - Nano-pillar array heterojunction and preparation method thereof - Google Patents
Nano-pillar array heterojunction and preparation method thereof Download PDFInfo
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- CN109950138B CN109950138B CN201910290197.XA CN201910290197A CN109950138B CN 109950138 B CN109950138 B CN 109950138B CN 201910290197 A CN201910290197 A CN 201910290197A CN 109950138 B CN109950138 B CN 109950138B
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- 239000002061 nanopillar Substances 0.000 title claims abstract description 23
- 238000002360 preparation method Methods 0.000 title claims abstract description 15
- 238000001704 evaporation Methods 0.000 claims abstract description 64
- 230000008020 evaporation Effects 0.000 claims abstract description 37
- 229910002899 Bi2Te3 Inorganic materials 0.000 claims abstract description 29
- 239000000758 substrate Substances 0.000 claims abstract description 24
- 229910017629 Sb2Te3 Inorganic materials 0.000 claims abstract description 22
- 238000002207 thermal evaporation Methods 0.000 claims abstract description 10
- 238000007738 vacuum evaporation Methods 0.000 claims abstract description 5
- 238000002156 mixing Methods 0.000 claims abstract description 3
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 6
- 239000011248 coating agent Substances 0.000 claims description 6
- 238000000576 coating method Methods 0.000 claims description 6
- 238000000034 method Methods 0.000 claims 6
- 229910052581 Si3N4 Inorganic materials 0.000 claims 1
- 238000004519 manufacturing process Methods 0.000 claims 1
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 claims 1
- 238000005516 engineering process Methods 0.000 abstract description 4
- 230000007547 defect Effects 0.000 abstract description 3
- 239000002086 nanomaterial Substances 0.000 abstract description 3
- 238000009826 distribution Methods 0.000 description 7
- 239000000463 material Substances 0.000 description 7
- 238000010586 diagram Methods 0.000 description 6
- 238000001816 cooling Methods 0.000 description 4
- 239000010408 film Substances 0.000 description 4
- 238000010438 heat treatment Methods 0.000 description 4
- 238000001000 micrograph Methods 0.000 description 4
- 239000000843 powder Substances 0.000 description 4
- 238000005086 pumping Methods 0.000 description 4
- 230000001105 regulatory effect Effects 0.000 description 4
- 238000005303 weighing Methods 0.000 description 4
- 239000013078 crystal Substances 0.000 description 2
- 238000001514 detection method Methods 0.000 description 2
- 239000002135 nanosheet Substances 0.000 description 2
- 238000010248 power generation Methods 0.000 description 2
- 238000005057 refrigeration Methods 0.000 description 2
- 239000004065 semiconductor Substances 0.000 description 2
- 238000004729 solvothermal method Methods 0.000 description 2
- 238000005411 Van der Waals force Methods 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000011229 interlayer Substances 0.000 description 1
- 239000010410 layer Substances 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000002073 nanorod Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 150000004772 tellurides Chemical class 0.000 description 1
- 239000010409 thin film Substances 0.000 description 1
- 238000007740 vapor deposition Methods 0.000 description 1
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Abstract
The invention relates to the technical field of nano structures, in particular to a nano column array heterojunction and a preparation method thereof. The invention provides a preparation method of a nano-pillar array heterojunction, which comprises the following steps: first opening Bi2Te3Evaporation source for evaporating Bi on substrate2Te3Then turn off Bi2Te3Evaporating source, then mixing Sb2Te3The evaporation source is turned on for vacuum evaporation and the product is collected on the substrate. The invention provides a nano-pillar array heterojunction and a preparation method thereof, and solves the technical defects that a one-dimensional nano-pillar array heterojunction is lacked and a vacuum thermal evaporation technology is utilized to prepare the nano-pillar array heterojunction in the prior art.
Description
Technical Field
The invention relates to the technical field of nano structures, in particular to a nano column array heterojunction and a preparation method thereof.
Background
Compounds of groups V-VI such as A2B3The material of (a) is widely used in the fields of thermoelectric power generation, thermoelectric refrigeration and the like because of its excellent thermoelectric properties, among which the properties of the telluride series material are excellent. At present, Bi is the most studied at home and abroad2Te3A composite material of the base.
Bi2Te3The material has excellent thermoelectric performance near room temperature, is widely used for refrigeration and power generation near room temperature, and is a room temperature thermoelectric material system widely applied in the thermoelectric materials at present in a commercialized way.
Sb2Te3The semiconductor material is also a semiconductor material belonging to a trigonal system, and the crystal thereof also has a layered structure with high symmetry, and adjacent layers are bonded by covalent bonds and interlayer are bonded by van der waals force, and the layered structure is advantageous for improving thermoelectric performance, and has excellent thermoelectric performance at room temperature, and thus has been spotlighted by extensive researchers.
Recent studies have shown that nanomaterials, because of their unique and excellent physicochemical properties, exhibit tremendous industrial applicationsHas great application value. Sb is synthesized by adopting solvothermal method by Songhenqi team of Wang Guangdong universities of Nanjing university2Te3/Bi2Te3Transverse heterojunction nanosheets, see Nano lett, 2015,15(9), pp 5905-; venkatasubramanian et al prepared Bi by metal organic vapor deposition2Te3/Sb2Te3Nano-superlattice thin films, see Journal of Crystal Growth,1997,170 (1): 817-821; t-type Bi prepared by Cheng et al by solvothermal method2T3-Te heterojunction comprising Bi of rhombohedral structure2Te3Te nanorods with nanosheet and trigonal structures are described in The Journal of Physical Chemistry C,2013,117(24):12458-12464.
The reports show that the research of the two-dimensional nano heterojunction is more, and the preparation method is more complex. The one-dimensional nano heterojunction can have unique performance due to small size, high surface-to-volume ratio and quantum confinement effect. Bi2Te3/Sb2Te3The heterojunction of the one-dimensional nano-column array is not reported, and the vacuum thermal evaporation technology is used for preparing Bi2Te3/Sb2Te3The nanopillar array heterojunction has not been reported yet.
Disclosure of Invention
The invention provides a nano-pillar array heterojunction and a preparation method thereof, and solves the technical defects that a one-dimensional nano-pillar array heterojunction is lacked and a vacuum thermal evaporation technology is utilized to prepare the nano-pillar array heterojunction in the prior art.
The invention provides a preparation method of a nano-pillar array heterojunction, which comprises the following steps:
first opening Bi2Te3Evaporation source for evaporating Bi on substrate2Te3Then turn off Bi2Te3Evaporating source, then mixing Sb2Te3The evaporation source is turned on for vacuum evaporation and the product is collected on the substrate.
Preferably, the substrate is a quartz glass substrate.
Preferably, Bi2Te3Evaporation source and Sb2Te3The evaporation source and the substrate are both 5cm apart.
Preferably, said Bi2Te3The temperature of the evaporation source was 520 ℃.
Preferably, said Sb is2Te3The temperature of the evaporation source was 550 ℃.
Preferably, said Bi2Te3The pressure intensity of evaporation source is 9 x 10-5Pa, said Sb2Te3The pressure intensity of evaporation source during evaporation is 7 x 10-5Pa。
Preferably, Bi2Te3Evaporation source and Sb2Te3The evaporation time of the evaporation source is 20 minutes.
Preferably, the vacuum evaporation equipment is a multi-source high-vacuum thermal evaporation coating machine.
The invention provides a nano-pillar array heterojunction, which is prepared by the preparation method.
Preferably, the shape of the nanopillar array heterojunction is a polygon.
The structure prepared by the preparation method provided by the embodiment of the invention has the advantages of compact surface, less gaps and obvious array structure. The experimental method is simple, has little pollution to the environment, is easy to operate and popularize, and can be used for large-area preparation, thereby having important research value and wide application prospect.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to these drawings without inventive exercise.
FIG. 1 is a scanning electron microscope image of the surface of a sample obtained in example 1 of the present invention;
FIG. 2 is a cross-sectional scanning electron microscope image of a sample obtained in example 1 of the present invention;
FIG. 3 is a distribution diagram of Bi element in the sample obtained in example 1 of the present invention;
FIG. 4 is a distribution diagram of Te element of a sample obtained in example 1 of the present invention;
FIG. 5 is a diagram showing the distribution of Sb elements in the sample obtained in example 1 of the present invention.
Detailed Description
The embodiment of the invention provides a nano-pillar array heterojunction and a preparation method thereof, and solves the technical defects that a one-dimensional nano-pillar array heterojunction is lacked and a vacuum thermal evaporation technology is utilized to prepare the nano-pillar array heterojunction in the prior art.
In order to make the objects, features and advantages of the present invention more obvious and understandable, the technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the accompanying drawings in the embodiments of the present invention, and it is obvious that the embodiments described below are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
Separately weighing Bi2Te3And Sb2Te3The molar ratio is 1: 1, respectively placing the powder in 2 different evaporation sources of a multi-source high-vacuum thermal evaporation coating machine, wherein the substrate is made of quartz glass, and the distance between the 2 evaporation sources and the substrate is adjusted to be 5 cm. The first stage, vacuum pumping to 9 × 10-5Pa, raising the substrate temperature to 250 ℃, and then raising Bi2Te3Evaporating for 20min when the evaporation source temperature reaches 520 ℃; second stage, turning off Bi2Te3Evaporation source, open Sb2Te3Evaporating, heating to 550 deg.C, and regulating pressure to 7 × 10- 5Pa, evaporating for 20 min. And cooling and collecting the product after the evaporation is finished.
Scanning electron microscope detection is carried out on the nano-pillar array heterojunction prepared in the embodiment 1 of the invention. As shown in fig. 1 and 2, fig. 1 is a surface scanning electron microscope image, and it can be seen that the sample surface is a continuous film composed of dense nano-scale grains. Fig. 2 is a cross-sectional scanning electron microscope image, which can clearly see the structure of the nanopillar array.
Element distribution detection is carried out on a part of the cross section of the nano-pillar array heterojunction prepared in the embodiment 1 of the invention. As shown in FIGS. 3 to 5, FIG. 3 is a distribution diagram of Bi element in the selected region, and it can be seen that the Bi element is uniformly distributed in the lower portion of the film. Fig. 4 is a distribution diagram of Te elements in selected areas, and it can be seen that Te elements are uniformly distributed in the film. Fig. 5 is a distribution diagram of Sb elements in selected regions, and it can be seen that Sb elements are uniformly distributed in the upper portion of the film. In summary, it can be seen that the upper half of the heterojunction of the nanopillar array is divided into Sb2Te3The lower half part is Bi2Te3。
Example 2
Separately weighing Bi2Te3And Sb2Te3The molar ratio is 1: 1, respectively placing the powder in 2 different evaporation sources of a multi-source high-vacuum thermal evaporation coating machine, wherein the substrate is made of quartz glass, and the distance between the 2 evaporation sources and the substrate is adjusted to be 5 cm. The first stage, vacuum pumping to 9 × 10-5Pa, raising the substrate temperature to 250 ℃, and then raising Bi2Te3Evaporating for 15min at the evaporation source temperature of 530 ℃; second stage, turning off Bi2Te3Evaporation source, open Sb2Te3Evaporating, heating to 550 deg.C, and regulating pressure to 7 × 10- 5Pa, evaporation for 15 min. And cooling and collecting the product after the evaporation is finished.
Example 3
Separately weighing Bi2Te3And Sb2Te3The molar ratio is 1: 1, respectively placing the powder in 2 different evaporation sources of a multi-source high-vacuum thermal evaporation coating machine, wherein the substrate is made of quartz glass, and the distance between the 2 evaporation sources and the substrate is adjusted to be 5 cm. The first stage, vacuum pumping to 9 × 10-5Pa, raising the substrate temperature to 230 ℃, and then raising Bi2Te3Evaporating for 20min when the evaporation source temperature reaches 500 ℃; second stage, turning off Bi2Te3Evaporation source, open Sb2Te3Evaporating, heating to 530 deg.C, and regulating pressure to 7 × 10- 5Pa, evaporating for 20 min. Cooling after evaporation is finished andthe product was collected.
Example 4
Separately weighing Bi2Te3And Sb2Te3The molar ratio is 1: 1, respectively placing the powder in 2 different evaporation sources of a multi-source high-vacuum thermal evaporation coating machine, wherein the substrate is made of quartz glass, and the distance between the 2 evaporation sources and the substrate is adjusted to be 5 cm. The first stage, vacuum pumping to 9 × 10-5Pa, raising the temperature of the substrate to 260 ℃, and then raising Bi2Te3Evaporating for 15min when the evaporation source temperature is 540 ℃; second stage, turning off Bi2Te3Evaporation source, open Sb2Te3Evaporating, heating to 570 deg.C, and regulating pressure to 7 × 10- 5Pa, evaporation for 15 min. And cooling and collecting the product after the evaporation is finished.
The above-mentioned embodiments are only used for illustrating the technical solutions of the present invention, and not for limiting the same; although the present invention has been described in detail with reference to the foregoing embodiments, it will be understood by those of ordinary skill in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some technical features may be equivalently replaced; and such modifications or substitutions do not depart from the spirit and scope of the corresponding technical solutions of the embodiments of the present invention.
Claims (10)
1. A preparation method of a nano-pillar array heterojunction is characterized by comprising the following steps:
first opening Bi2Te3Evaporation source for evaporating Bi on substrate2Te3Then turn off Bi2Te3Evaporating source, then mixing Sb2Te3The evaporation source is turned on for vacuum evaporation and the product is collected on the substrate.
2. The production method according to claim 1, wherein the substrate is a quartz glass substrate.
3. The method according to claim 1, wherein Bi2Te3Evaporation ofSource and Sb2Te3The evaporation source and the substrate are both 5cm apart.
4. The method according to claim 1, wherein said Bi is2Te3The temperature of the evaporation source was 520 ℃.
5. The method according to claim 1, wherein the Sb is2Te3The temperature of the evaporation source was 550 ℃.
6. The method according to claim 1, wherein said Bi is2Te3The pressure intensity of evaporation source is 9 x 10-5Pa, said Sb2Te3The pressure intensity of evaporation source during evaporation is 7 x 10-5Pa。
7. The method according to claim 1, wherein Bi2Te3Evaporation source and Sb2Te3The evaporation time of the evaporation source is 20 minutes.
8. The method for preparing the silicon nitride film according to the claim 1, wherein the vacuum evaporation equipment is a multi-source high vacuum thermal evaporation coating machine.
9. A nanopillar array heterojunction, characterized in that it is prepared by the preparation method of any one of claims 1 to 7.
10. The nanopillar array heterojunction as claimed in claim 9 wherein the shape is polygonal.
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| US7888583B2 (en) * | 2007-05-07 | 2011-02-15 | Wisconsin Alumni Research Foundation | Semiconductor nanowire thermoelectric materials and devices, and processes for producing same |
| CN201156551Y (en) * | 2008-02-26 | 2008-11-26 | 杭州电子科技大学 | Nano pyroelectric material of core-shell construction |
| CN101434455B (en) * | 2008-12-01 | 2011-01-12 | 北京航空航天大学 | Method for preparing bismuth telluride nano-wire array by physical vapour deposition |
| KR101047610B1 (en) * | 2009-10-15 | 2011-07-07 | 연세대학교 산학협력단 | Method for manufacturing thermoelectric nanowires having a core / shell structure |
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