CN109881247B - Preparation method of bent SnTe single crystal nanowire - Google Patents
Preparation method of bent SnTe single crystal nanowire Download PDFInfo
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- CN109881247B CN109881247B CN201910194043.0A CN201910194043A CN109881247B CN 109881247 B CN109881247 B CN 109881247B CN 201910194043 A CN201910194043 A CN 201910194043A CN 109881247 B CN109881247 B CN 109881247B
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- 239000002070 nanowire Substances 0.000 title claims abstract description 71
- 229910005642 SnTe Inorganic materials 0.000 title claims abstract description 53
- 239000013078 crystal Substances 0.000 title claims abstract description 30
- 238000002360 preparation method Methods 0.000 title claims abstract description 15
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 36
- 239000010453 quartz Substances 0.000 claims abstract description 30
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- 238000010438 heat treatment Methods 0.000 claims abstract description 25
- 239000000843 powder Substances 0.000 claims abstract description 20
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims abstract description 16
- 239000007789 gas Substances 0.000 claims abstract description 16
- 239000012159 carrier gas Substances 0.000 claims abstract description 14
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 claims abstract description 10
- 239000010931 gold Substances 0.000 claims abstract description 10
- 229910052737 gold Inorganic materials 0.000 claims abstract description 10
- 229910052786 argon Inorganic materials 0.000 claims abstract description 8
- 229910052681 coesite Inorganic materials 0.000 claims abstract description 6
- 229910052906 cristobalite Inorganic materials 0.000 claims abstract description 6
- 239000000377 silicon dioxide Substances 0.000 claims abstract description 6
- 229910052682 stishovite Inorganic materials 0.000 claims abstract description 6
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- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 6
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 6
- 239000012153 distilled water Substances 0.000 claims description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 4
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 3
- 239000001307 helium Substances 0.000 claims description 3
- 229910052734 helium Inorganic materials 0.000 claims description 3
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 claims description 3
- 229910052754 neon Inorganic materials 0.000 claims description 3
- GKAOGPIIYCISHV-UHFFFAOYSA-N neon atom Chemical compound [Ne] GKAOGPIIYCISHV-UHFFFAOYSA-N 0.000 claims description 3
- 229910052757 nitrogen Inorganic materials 0.000 claims description 3
- 238000001771 vacuum deposition Methods 0.000 claims description 3
- 239000007888 film coating Substances 0.000 claims description 2
- 238000009501 film coating Methods 0.000 claims description 2
- 238000004506 ultrasonic cleaning Methods 0.000 claims description 2
- 238000005229 chemical vapour deposition Methods 0.000 description 12
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- 239000012212 insulator Substances 0.000 description 2
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- 239000000956 alloy Substances 0.000 description 1
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- MFIWAIVSOUGHLI-UHFFFAOYSA-N selenium;tin Chemical compound [Sn]=[Se] MFIWAIVSOUGHLI-UHFFFAOYSA-N 0.000 description 1
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- WYUZTTNXJUJWQQ-UHFFFAOYSA-N tin telluride Chemical compound [Te]=[Sn] WYUZTTNXJUJWQQ-UHFFFAOYSA-N 0.000 description 1
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Abstract
The invention discloses a preparation method of a bent SnTe single crystal nanowire, which comprises the following steps: in Si/SiO2Plating a layer of gold film on the surface of the sheet as a substrate; putting the substrate and the SnTe powder source into a quartz tube, putting the quartz tube into a tubular heating furnace, and exhausting air in the tubular heating furnace in a repeated inflation and exhaust mode by using gas which does not participate in reaction as cleaning gas; argon is used as carrier gas, SnTe powder is positioned in the middle of a heating furnace, a substrate is positioned at the downstream of the flowing of the carrier gas, a tubular heating furnace is started to heat and raise the temperature, and nanowires grow under a growing condition; moving the tubular heating furnace to the downstream of the carrier gas flow for a certain distance, and continuing to grow the nanowires of the bent part under the same growth conditions; and naturally cooling to obtain the bent SnTe single crystal nanowire.
Description
Technical Field
The invention belongs to the technical field of nano material preparation, and particularly relates to a preparation method of a bent SnTe (tin telluride) single crystal nanowire based on a vapor deposition method.
Background
Topological crystal insulators are the hot spot of recent research on nano-quantum materials, possessing non-trivial energy gap-free conducting surface states (topological surface states) and insulating bulk states, which are protected by crystal plane symmetry. SnTe is a typical topological crystalline insulator material, theoretical calculation shows that topological states related to crystal planes exist in the SnTe material, and a typical quantum effect in SnTe nanowires is detected experimentally, so that the existence of a topological surface state without energy gaps is proved. The SnTe nanowire has topological properties, so that the SnTe nanowire can be applied to the fields of non-dissipative quantum computing devices, spintronic devices and the like, and has high research value.
The gas-liquid-solid growth mechanism is a mechanism widely applied to preparation of one-dimensional nano materials, and is proposed by Wanger and Ellis in the research of the growth process of Si nanowires in 1964, and the catalyst liquid drop is considered to play a crucial role in the growth process of Si whiskers, and Givardizov is analyzed from the growth dynamics in 1975 to further explain some complex phenomena in the growth process of Si nanowires and perfect the gas-liquid-solid growth mechanism. The basic principle of the gas-liquid-solid growth mechanism is as follows: the gas phase reactant flows above the catalyst liquid drop along with the carrier gas and is dissolved in the catalyst liquid drop, and the catalyst liquid drop reaches a supersaturated state in a short time, so that the catalyst liquid drop is nucleated and grows on a liquid-solid reaction interface, thereby obtaining the nanowire. In many current nanowire material preparation studies, most nanowires can grow through a gas-liquid-solid growth mechanism, and before the mechanism is used, phase diagrams of some simple alloys of reactant phases need to be studied, so that a proper catalyst material can be found. In addition, when the nanowire grows by using a gas-liquid-solid growth mechanism, the nanowire can grow only to one dimension by using the action of the catalyst, so that the diameter and the surface appearance of the nanowire are controlled. Meanwhile, researches show that in the process of growing the nanowire by a gas-liquid-solid growth mechanism, a mutual competitive relationship between axial growth and radial growth possibly exists, and the radial growth mode is a gas-solid growth mechanism.
At present, there are many methods for preparing nano materials, and several methods mainly used for research and application include chemical vapor deposition, molecular beam epitaxy, metal organic chemical vapor deposition, chemical beam epitaxy and the like. The chemical vapor deposition method is a commonly used method for preparing nano materials, namely, a gas source substance is directly utilized or indirectly changed into a gas precursor by heating and other modes, and the gas is decomposed, combined or otherwise reacted under the action of external conditions to obtain the nano materials on a substrate. The molecular beam epitaxy method is characterized in that in an ultrahigh vacuum equipment environment, a source material is fully evaporated by using a high-temperature or electron beam heating means to generate a large amount of molecular beams, the strength of the molecular beams is controlled by using a high-precision control means, and then the molecular beams are sprayed onto a corresponding proper substrate, so that the epitaxial growth of a nano material is realized. The method can control the low-speed growth of the nano-wire and effectively reduce lattice defects, but has high requirements on equipment. With the progress of research, a metal organic chemical vapor deposition method is developed on the basis of a chemical vapor deposition method, and a metal organic compound is adopted as a precursor of the metal organic chemical vapor deposition method, so that the metal organic chemical vapor deposition method is more applied to preparing III-V group semiconductor nanowires. Chemical beam epitaxy combines the advantages of metal organic chemical vapor deposition and molecular beam epitaxy, and is one new type of epitaxial growth process for growing film material on substrate. Both of these methods have a serious drawback in that the source materials are generally extremely toxic and are not suitable for research and application.
Compared with other methods, the chemical vapor deposition method has the advantages of simple equipment, low research cost, simple and convenient research process and the like, so the method is widely applied to the preparation of various nano materials. For example, the chinese invention patent CN105399061A discloses a method for preparing a one-dimensional tin selenide single crystal nanowire, which comprises placing SnSe powder in a high temperature resistant container, placing the SnSe powder at the position of the furnace mouth of a vacuum tube furnace, placing a substrate material attached with a catalyst in the high temperature resistant furnace tube, introducing a protective gas in an oxygen-free vacuum state for heating, moving the high temperature resistant furnace tube to make the high temperature container located in a central high temperature region and the substrate attached with the catalyst located in a low temperature region, and growing the one-dimensional SnSe single crystal nanowire. However, the high temperature resistant furnace tube is moved in the method only for providing proper nanowire growth conditions, and the method can only be used for growing linear SnSe single crystal nanowires and cannot obtain SnTe single crystal nanowires with bent structures.
Disclosure of Invention
The invention aims to provide a preparation method of a bent SnTe single crystal nanowire, which is based on a chemical vapor deposition method, adopts a simple chemical vapor deposition equipment system, and can grow the bent SnTe single crystal nanowire without other complicated operation and control means.
In order to achieve the purpose, the invention adopts the following technical scheme:
a preparation method of a bent SnTe single-crystal nanowire comprises the following steps:
in Si/SiO2Plating a layer of gold film on the surface of the sheet as a substrate;
putting the substrate and the SnTe powder source into a quartz tube, putting the quartz tube into a tubular heating furnace, and exhausting air in the tubular heating furnace in a repeated inflation and exhaust mode by using gas which does not participate in reaction as cleaning gas;
argon is used as carrier gas, SnTe powder is positioned in the middle of a heating furnace, a substrate is positioned at the downstream of the flowing of the carrier gas, a tubular heating furnace is started to heat and raise the temperature, and nanowires grow under a growing condition;
moving the tubular heating furnace to the downstream of the carrier gas flow for a certain distance, and continuing to grow the nanowires of the bent part under the same growth conditions;
and naturally cooling to obtain the bent SnTe single crystal nanowire.
Further, Si/SiO2The sheet is firstly put into acetone, absolute ethyl alcohol and distilled water in sequence for ultrasonic cleaning respectively, then taken out and dried by high-pressure nitrogen, and then put into an evaporative vacuum coating machine for gold film coating.
Further, the thickness of the gold film is 2-4 nm.
Further, the substrate was placed in a quartz tile and the quartz tile was placed in a quartz tube.
Further, SnTe powder was placed in a quartz boat, and then the quartz boat was placed in a quartz tube.
Further, the gas not participating in the reaction includes helium, neon, argon.
Further, the growth condition is that the growth is kept for 14-16 min at 18-22 kPa and 690-710 ℃.
Further, the growth conditions are preferably 20kPa at 700 ℃ for 15 min.
Further, the distance between the substrate and the SnTe powder is 14.5-15.5 cm.
Further, the moving distance is 0.8-1 cm.
Further, the distance of the movement is preferably 1 cm.
The bent SnTe single-crystal nanowire prepared by the method.
The substrate and the SnTe powder source are put into a chemical vapor deposition equipment system, and the simple operation of moving the furnace is carried out in the heating growth stage, so that the SnTe bent nanowire is grown. The growth of the SnTe nano wire comprises two stages, wherein the first stage is adopted before the movement of the tubular heating furnace, and the temperature of the first stage is enough to provide the growth conditions of the nano wire; and the moving tube type heating furnace provides an instantaneous variable for the growth of the nanowire at the second stage, and the growth direction of the nanowire is changed, so that the bent part of the nanowire is grown, and the SnTe single crystal nanowire with the bent structure is obtained. Therefore, the method can obtain the bent SnTe single crystal nanowire by simple operation without other complicated operation and control means.
Drawings
FIG. 1 is a schematic view of the growth of a bent SnTe single-crystal nanowire in the example.
In the figure: 1-tubular heating furnace, 2-slide rail, 3-quartz tube, 4-SnTe powder, 5-quartz boat, 6-substrate, 7-quartz tile.
Fig. 2 is a typical SnTe bent nanowire growth temperature set-up curve, set-up temperature of 700 ℃.
Fig. 3A is an electron microscope image of a SnTe bent nanowire grown on a substrate, and the insert at the upper right corner is an electron microscope image of a single bent nanowire.
Fig. 3B is a transmission electron microscope image of a single bent nanowire, wherein the bend of the nanowire is 90 °.
Fig. 4A is an X-ray energy spectrum of the dashed area in fig. 3B, which is used to measure the elemental composition and ratio of the area.
Fig. 4B is an X-ray energy spectrum of the solid-line frame region of fig. 3B, which is used to measure the elemental composition and proportion of the region.
FIG. 5A is a high resolution TEM image of the solid line frame region of FIG. 3B, with an electron diffraction pattern selected from the top-right inset.
FIG. 5B is a high resolution TEM image of the dashed area of FIG. 3B, with an electron diffraction pattern selected from the top-right inset.
FIG. 5C is a TEM high resolution image of the outside of the nanowire kink in FIG. 3B, with an inset in the top right hand corner showing a selected electron diffraction pattern.
FIG. 5D is a TEM high resolution image of the inside of the nanowire kink in FIG. 3B, with an inset in the top right corner showing a selected electron diffraction pattern.
Detailed Description
In order to make the aforementioned and other features and advantages of the invention more comprehensible, embodiments accompanied with figures are described in detail below.
Example 1
The embodiment discloses a preparation method of a bent SnTe single crystal nanowire, which comprises the following steps:
experimental materials and equipment:
quartz tube, quartz boat, quartz tile, Si/SiO2Slice, SnTe powder, high pressure argon, mechanical pump.
The experimental steps are as follows:
1. substrate preparation
4 inches of Si/SiO2And putting the slices into acetone, absolute ethyl alcohol and distilled water in sequence, performing ultrasonic treatment for 5min, taking out the slices, and blowing the distilled water on the surface by using a high-pressure nitrogen gun. Then the cleaned wafer is put into an evaporative vacuum coating machine, and a layer of gold film with the thickness of 3nm is coated on the surface of the wafer. Finally, the coated wafer was cut with a diamond knife and cut into a substrate of 5mm × 5 mm.
2. Preparation of prophase growth
As shown in figure 1, the invention adopts SnTe powder as a growth source, 0.2g of SnTe powder is weighed and placed in a quartz boat (with the length of 2cm, the outer diameter of 10mm and the inner diameter of 8mm), and the quartz boat is placed in a quartz tube, and the position of the quartz boat is flush with the center of the tube furnace; the prepared substrate was placed in a quartz tile (length 10cm, outer diameter 10mm, inner diameter 8mm) and the tile was then placed in a quartz tube (length 120cm, outer diameter 25mm, inner diameter 23mm) with the tile downstream flush with one end of the tube furnace and the substrate 15cm from the powder source. Finally, the whole growth system is sealed, argon is used as cleaning gas, and air is pumped by combining a mechanical pump, so that air in the whole system is exhausted, and the limiting pressure can reach 10 Pa.
3. Growth process
As shown in fig. 1, after the preparation step of the early stage of growth is completed, the tube furnace is started, the target temperature is set to 700 ℃, and argon is used as carrier gas. Fig. 2 is a typical SnTe bent nanowire growth temperature set-up curve, set-up temperature of 700 ℃. The whole growth process is divided into 2 stages: (1) heating in a tube furnace to 700 deg.C, and maintaining for 15 min; (2) and after 15min, moving the tube furnace 1cm towards the downstream where the carrier gas flows, continuously maintaining the tube furnace at 700 ℃ for heat preservation for 15min, then naturally cooling, and keeping the system pressure in the whole process at 20kPa to obtain the SnTe single crystal nanowire bent at 90 degrees.
Fig. 3A is an electron microscope image of a SnTe bent nanowire grown on a substrate, and the insert at the upper right corner is an electron microscope image of a single bent nanowire. Fig. 3B is a transmission electron microscope image of a single bent nanowire, wherein the bend of the nanowire is 90 °. As can be seen from the attached drawings, the SnTe bent nanowire is successfully prepared by the method.
Fig. 4A is an X-ray energy spectrum of the dashed area in fig. 3B, which is used to measure the elemental composition and ratio of the area. Fig. 4B is an X-ray energy spectrum of the solid-line frame region of fig. 3B, which is used to measure the elemental composition and proportion of the region. FIG. 5A is a high resolution TEM image of the solid line frame region of FIG. 3B, with an electron diffraction pattern selected from the top-right inset. FIG. 5B is a high resolution TEM image of the dashed area of FIG. 3B, with an electron diffraction pattern selected from the top-right inset. FIG. 5C is a TEM high resolution image of the outside of the nanowire kink in FIG. 3B, with an inset in the top right hand corner showing a selected electron diffraction pattern. FIG. 5D is a TEM high resolution image of the inside of the nanowire kink in FIG. 3B, with an inset in the top right corner showing a selected electron diffraction pattern. As can be seen from the drawings, the SnTe bent nanowire with the single crystal structure is successfully prepared by the method.
Example 2
This example discloses a method for preparing a bent SnTe single crystal nanowire, which is substantially the same as example 1, except that the thickness of the gold film is 2nm, helium is selected as a gas not participating in the reaction, the nanowire growth conditions are selected to be maintained at 18kPa and 690 ℃ for 16min, the distance between the substrate and the SnTe powder is 14.5cm, and the downstream movement distance of the tubular heating furnace to the carrier gas flow is 0.9 cm. In this example, the bent SnTe single crystal nanowire is also successfully prepared.
Example 3
This example discloses a method for preparing a bent SnTe single crystal nanowire, which is substantially the same as example 1, except that the thickness of the gold film is 4nm, the gas not participating in the reaction is neon, the nanowire growth conditions are selected to be maintained at 22kPa and 710 ℃ for 14min, the distance between the substrate and the SnTe powder is 15.5cm, and the downstream movement distance from the tubular heating furnace to the flow of the carrier gas is 0.8 cm. In this example, the bent SnTe single crystal nanowire is also successfully prepared.
The above embodiments are only intended to illustrate the technical solution of the present invention and not to limit the same, and a person skilled in the art can modify the technical solution of the present invention or substitute the same without departing from the spirit and scope of the present invention, and the scope of the present invention should be determined by the claims.
Claims (9)
1. A preparation method of a bent SnTe single crystal nanowire is characterized by comprising the following steps:
in Si/SiO2Plating a layer of gold film on the surface of the sheet as a substrate;
putting the substrate and the SnTe powder source into a quartz tube, putting the quartz tube into a tubular heating furnace, and exhausting air in the tubular heating furnace in a repeated inflation and exhaust mode by using gas which does not participate in reaction as cleaning gas;
argon is used as carrier gas, SnTe powder is positioned in the middle of a heating furnace, a substrate is positioned at the downstream of the flowing of the carrier gas, a tubular heating furnace is started to heat and raise the temperature, and nanowires grow under a growing condition;
moving the tubular heating furnace to the downstream of the carrier gas flow by 0.8-1 cm, and continuing to grow the nanowires of the bent part under the same growth conditions;
and naturally cooling to obtain the bent SnTe single crystal nanowire.
2. The method of claim 1, wherein the Si/SiO is2The sheet is firstly put into acetone, absolute ethyl alcohol and distilled water in sequence for ultrasonic cleaning respectively, then taken out and dried by high-pressure nitrogen, and then put into an evaporative vacuum coating machine for gold film coating.
3. The method of claim 1 or 2, wherein the gold film has a thickness of 2 to 4 nm.
4. The method of claim 1, wherein the substrate is placed in a quartz tile and the quartz tile is placed in a quartz tube; the SnTe powder is firstly put into a quartz boat, and then the quartz boat is put into a quartz tube.
5. The method of claim 1, wherein the non-reactive gas comprises helium, neon, or argon.
6. The method according to claim 1, wherein the growth conditions are 18 to 22kPa at 690 to 710 ℃ for 14 to 16 min.
7. The method according to claim 6, wherein the growth conditions are preferably 20kPa, 700 ℃ for 15 min.
8. The method of claim 1, wherein the substrate is at a distance of 14.5-15.5 cm from the SnTe powder.
9. A bent SnTe single-crystal nanowire prepared by the method as claimed in any one of claims 1 to 8.
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