CN117623236A - Bismuth selenide (BiSe) nanowire/nano-ribbon and preparation method thereof - Google Patents
Bismuth selenide (BiSe) nanowire/nano-ribbon and preparation method thereof Download PDFInfo
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- 239000002070 nanowire Substances 0.000 title claims abstract description 63
- 238000002360 preparation method Methods 0.000 title claims abstract description 26
- FBGGJHZVZAAUKJ-UHFFFAOYSA-N bismuth selenide Chemical compound [Se-2].[Se-2].[Se-2].[Bi+3].[Bi+3] FBGGJHZVZAAUKJ-UHFFFAOYSA-N 0.000 title claims abstract 28
- 239000002074 nanoribbon Substances 0.000 title abstract description 23
- 239000002127 nanobelt Substances 0.000 claims abstract description 38
- 239000000758 substrate Substances 0.000 claims abstract description 37
- 239000010453 quartz Substances 0.000 claims abstract description 34
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 34
- 239000000843 powder Substances 0.000 claims abstract description 29
- 238000007747 plating Methods 0.000 claims abstract description 23
- 239000007789 gas Substances 0.000 claims abstract description 17
- 238000000034 method Methods 0.000 claims abstract description 13
- 239000012159 carrier gas Substances 0.000 claims abstract description 7
- 238000005229 chemical vapour deposition Methods 0.000 claims abstract description 7
- 238000006243 chemical reaction Methods 0.000 claims description 21
- 238000010438 heat treatment Methods 0.000 claims description 6
- 230000035484 reaction time Effects 0.000 claims description 5
- 238000011144 upstream manufacturing Methods 0.000 claims description 3
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 2
- 239000001301 oxygen Substances 0.000 claims description 2
- 229910052760 oxygen Inorganic materials 0.000 claims description 2
- 238000003912 environmental pollution Methods 0.000 abstract description 2
- 229910010272 inorganic material Inorganic materials 0.000 abstract description 2
- 239000011147 inorganic material Substances 0.000 abstract description 2
- 238000011160 research Methods 0.000 abstract description 2
- OMEPJWROJCQMMU-UHFFFAOYSA-N selanylidenebismuth;selenium Chemical compound [Se].[Bi]=[Se].[Bi]=[Se] OMEPJWROJCQMMU-UHFFFAOYSA-N 0.000 description 72
- 239000010408 film Substances 0.000 description 17
- 230000000052 comparative effect Effects 0.000 description 10
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- 239000004065 semiconductor Substances 0.000 description 2
- 238000002207 thermal evaporation Methods 0.000 description 2
- 239000010409 thin film Substances 0.000 description 2
- AFCARXCZXQIEQB-UHFFFAOYSA-N N-[3-oxo-3-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)propyl]-2-[[3-(trifluoromethoxy)phenyl]methylamino]pyrimidine-5-carboxamide Chemical compound O=C(CCNC(=O)C=1C=NC(=NC=1)NCC1=CC(=CC=C1)OC(F)(F)F)N1CC2=C(CC1)NN=N2 AFCARXCZXQIEQB-UHFFFAOYSA-N 0.000 description 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- 230000004075 alteration Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
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- 229910052594 sapphire Inorganic materials 0.000 description 1
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- 229910052710 silicon Inorganic materials 0.000 description 1
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Abstract
The invention belongs to the technical field of inorganic materials, and particularly relates to a bismuth selenide (BiSe) nanowire/nanobelt and a preparation method thereof. The invention provides a preparation method of bismuth selenide (BiSe) nanowires/nanobelts, which utilizes a simple chemical vapor deposition method by using Bi 2 Se 3 The powder and Bi powder are used as growth sources, quartz plates with or without Au plating films are used as growth substrates, and the quartz plates are heated to a certain temperature under the condition that rare gas is used as carrier gas and then reacted to prepare the Au-plated quartz plate. Meanwhile, the prepared bismuth selenide (BiSe) nanowire/nanoribbon has regular shape and typical one-dimensional characteristics. In addition, the preparation method disclosed by the invention is simple in steps, can be used for rapid mass preparation, is high in product purity, has small environmental pollution, and is easy to operate and popularize, so that the preparation method has important research value and wide application prospect.
Description
Technical Field
The invention belongs to the technical field of inorganic materials, and particularly relates to a bismuth selenide (BiSe) nanowire/nanobelt and a preparation method thereof.
Background
In recent years, with the development of low-dimensional materials, many materials with nanostructures (such as two-dimensional thin films and one-dimensional nanowires) have been researched and found to have better special properties than bulk materials. Wherein, (Bi) 2 )m(Bi 2 Se 3 ) The topological insulating material of n (m, n are integers) series has typical penta-sublayer Se-Bi-Se (Bi 2 Se 3 ) And Bi-layer Bi-Bi (Bi) 2 ) A layered heterostructure is formed. But with Bi 2 Se 3 (m=0, n=1), the BiSe (m=1, n=2) is provided with Bi 2 Double layers, rather than being formed by repeated stacking of a single pentagenic layer Bi-Se-Bi, are considered potential new near room temperature thermoelectric materials due to their special crystal structure and excellent electrical transport properties.
For topological insulators, in order to avoid the influence of the body state on the surface state, the nano structure with high specific surface area is a good choice for researching topological properties, so that the preparation of nano materials is particularly important. Up to now, (Bi) 2 )m(Bi 2 Se 3 ) The preparation of n-type topological insulating nano materials has advanced to some extent. For example, there is a study on the growth of Bi with a flat surface morphology and a small height difference in a wide range of 2 μm on a sapphire substrate by using a molecular epitaxy apparatus 2 Se 3 A film. Also studied are the preparation of Bi having a diameter of about 410nm and a length of 20 to 200 μm on a silicon substrate by a VLS mechanism by thermal evaporation 2 Se 3 A nanowire. There have also been studies on the use of vacuum thermal evaporation to grow a BiSe thin film having a thickness of about 500nm and a crystal grain in a sheet-like shape on a high vacuum coater. However, at present (Bi 2 )m(Bi 2 Se 3 ) The n-type topological insulating nano material is a multi-dimensional nano structure, and has not been reported for the growth of one-dimensional BiSe nanowires/nanobelts. Moreover, the one-dimensional nano structure has special physical properties compared with the conventional size material, so that the application range of the material is expected to be further expanded. Therefore, the development of BiSe with typical one-dimensional characteristics has important application prospect.
Disclosure of Invention
In order to overcome the defects in the prior art, the invention provides a preparation method of bismuth selenide (BiSe) nanowires/nanobelts, and the prepared (BiSe) nanowires/nanobelts have regular shapes, have typical one-dimensional characteristics, improve the physical properties and enlarge the application range.
In order to achieve the above purpose, the technical scheme adopted by the invention is as follows:
the first aspect of the present invention provides a method for preparing bismuth selenide (BiSe) nanowires/nanobelts, comprising the steps of:
s1, bi 2 Se 3 Powder and Bi powder are used as growth sources, quartz plates with or without Au plating are used as growth substrates, and then Bi is used as a growth substrate 2 Se 3 Placing the powder in a heating center of a reaction area of the chemical vapor deposition equipment, placing Bi powder on the upstream of the heating center, and placing a quartz substrate on the downstream of the heating center;
s2, removing oxygen in the reaction area, inputting rare gas as carrier gas, maintaining the air pressure of the reaction area within a certain range, and heating to a certain temperature for reaction to prepare the bismuth selenide (BiSe) nanowire/nanobelt.
The invention uses a simple chemical vapor deposition method by using Bi 2 Se 3 The powder and Bi powder are used as growth sources, quartz plates with or without Au plating films are used as growth substrates, and the bismuth selenide (BiSe) nanowire/nanoribbon is prepared by heating to a certain temperature under the condition of taking rare gas as carrier gas and then reacting. In the invention, whether Au plating film treatment is carried out on the quartz substrate is selected, and the experimental growth effects are different. Wherein, compared with the growth effect of the quartz substrate without the Au plating film treatment, the quartz substrate with the Au plating film treatment grows more and more dense BiSe nanowires/nanobelts.
Preferably, in step S1, the Bi 2 Se 3 The mass ratio of the powder to the Bi powder is 1:1.
Preferably, in the step S1, the Bi powder is 2-10 cm away from the heating center, the quartz substrate without the Au plating film is 9-14 cm away from the heating center, and the quartz substrate with the Au plating film is 9-11 cm away from the heating center.
More preferably, the quartz substrate without the Au plating film is 9 to 12cm from the heating center, and the quartz substrate with the Au plating film is 9 to 10cm from the heating center.
Preferably, in step S2, the reaction temperature is 640-680 ℃ and the reaction time is 0.5-6 h.
More preferably, the reaction temperature is 640-680℃and the reaction time is 1-2 hours.
Preferably, in step S2, the rare gas includes Ar gas, and the gas flow is controlled to be 50-100 sccm.
Preferably, in step S2, the gas pressure in the reaction region is maintained at 150Pa or less.
In a second aspect, the present invention provides bismuth selenide (BiSe) nanowires/nanobelts prepared by the preparation method described in the first aspect.
The chemical formula of the bismuth selenide nanowire/nano-belt prepared by the invention is BiSe, which belongs to (Bi) 2 ) m (Bi 2 Se 3 ) n A compound wherein m=1, n=2. Meanwhile, the prepared (BiSe) nanowire/nanoribbon has regular shape and typical one-dimensional characteristics, the length of the nanowire/nanoribbon is 10-300 mu m, the diameter is 200-800 nm, and the larger length-diameter ratio improves the physical property of the nanowire/nanoribbon, so that the application range of the nanowire/nanoribbon is expanded, and the application prospect is wide.
Compared with the prior art, the invention has the beneficial effects that:
the invention provides a preparation method of bismuth selenide (BiSe) nanowires/nanobelts, which uses Bi 2 Se 3 The powder and Bi powder are used as growth sources, a quartz plate with or without an Au plating film is used as a growth substrate, the distance between the quartz substrate and a heating center is regulated, and then the quartz substrate is heated to a certain temperature under the condition that rare gas is used as carrier gas for reaction, so that the Au plating film is prepared. The prepared (BiSe) nanowire/nanoribbon has regular shape and typical one-dimensional characteristics. Meanwhile, the length of the obtained (BiSe) nanowire/nanoribbon is 10-300 mu m, the diameter is 200-800 nm, and the larger length-diameter ratio improves the physical property of the nanowire/nanoribbon, so that the application range of the nanowire/nanoribbon is enlarged (the semiconductor material with the one-dimensional structure with the larger length-diameter ratio can be better applied to a nanoscale semiconductor device, and the device performance is improved). In addition, the process for growing the bismuth selenide (BiSe) nanowire/nanoribbon by adopting the chemical vapor deposition method has the advantages of simple steps, easy operation and popularization, high product purity, rapid and large-scale preparation and small environmental pollution, thereby having important research value and wide application prospect.
Drawings
FIG. 1 is an X-ray diffraction pattern of bismuth selenide (BiSe) nanowires/nanobelts of examples 1, 2;
FIG. 2 is Bi of comparative example 1 2 Se 3 X-ray diffraction pattern of (2);
FIG. 3 is a scanning electron microscope image of bismuth selenide (BiSe) nanowires/nanobelts of example 1;
FIG. 4 is a scanning electron microscope image of bismuth selenide (BiSe) nanowires/nanobelts of example 2;
FIG. 5 is a scanned image of bismuth selenide (BiSe) nanowires/nanobelts and EDS spectra of example 1;
fig. 6 is a scanned image of bismuth selenide (BiSe) nanowires/nanobelts and EDS spectra of example 2.
Detailed Description
The following describes the invention in more detail. The description of these embodiments is provided to assist understanding of the present invention, but is not intended to limit the present invention. In addition, the technical features of the embodiments of the present invention described below may be combined with each other as long as they do not collide with each other.
The experimental methods in the following examples, unless otherwise specified, are conventional, and the experimental materials used in the following examples, unless otherwise specified, are commercially available.
Example 1
(1) Weighing 0.2g of Bi powder and 0.2g of Bi 2 Se 3 Respectively placing the powder on different arks as growth sources, and placing a plurality of cleaned quartz substrates without Au plating film treatment on the inverted arks as growth substrates;
(2) Will be provided with Bi 2 Se 3 Placing the powder ark in a heating center of a reaction device (chemical vapor deposition equipment, instrument name: high temperature tube furnace, model: GSL-1700X, manufacturer: hefei Kogyo materials technology Co., ltd.) tube furnace, placing the powder ark containing Bi powder on the upstream of the heating center, 3cm away from the heating center, and placing the inverted ark with quartz substrate on the downstream of the heating center, wherein the quartz substrate is 9-14 cm away from the heating center (9, 10, 11, 12, 13, 14cm respectively);
(3) Closing the flange, opening the mechanical pump to vacuumize the reaction device, then introducing carrier gas Ar gas, adjusting the gas flow to 70sccm, and maintaining the vacuum indication below 150 pa;
(4) Setting the heating rate to be 10 ℃/min, heating to 650 ℃, preserving heat for 2 hours, cooling to room temperature along with a furnace, closing a heating switch and gas, and taking out a sample to obtain the BiSe nanowire/nanobelt.
X-ray diffraction analysis is carried out on the bismuth selenide (BiSe) nanowire/nanobelt prepared in the example 1, the analysis result is shown as B1 in the figure 1, and the product has good crystallinity and obvious orientation; and the main phases of the samples are matched with BiSe (PDF#29-0246), and the strong diffraction peaks correspond to (005) and (0012) crystal faces, so that the purity of the synthesized product is high.
The bismuth selenide (BiSe) nanowire/nanoribbon prepared in example 1 was subjected to scanning electron microscope analysis, the analysis result is shown in fig. 3, the product length range is about 50-300 μm as seen in fig. 3 (a), and the product is nanowire (b) and nanoribbon (c) with obvious one-dimensional characteristics as seen in fig. 3 (b) and (c), and the shape is regular.
The bismuth selenide (BiSe) nanowire/nanoribbon prepared in example 1 was subjected to electron microscope scanning and EDS (electron beam ionization) energy spectrum test, the test results are shown in fig. 5, fig. 5 shows EDS (electron beam ionization) energy spectrum images corresponding to the bismuth selenide (BiSe) nanowire/nanoribbon and the detected atomic ratio, and the result shows that the atomic ratio of Bi to Se is 49.55:50.45, and is close to the standard atomic ratio of BiSe of 1:1.
Example 2
The preparation method is the same as in example 1, except that: the quartz substrate without Au plating film treatment in example 1 was replaced with an Au plating film quartz substrate, and an inverted ark with the quartz substrate was placed downstream of the heating center, 9 to 11cm (9, 10, 11cm, respectively) from the heating center, and a BiSe nanowire/nanoribbon was grown.
X-ray diffraction analysis is carried out on the bismuth selenide (BiSe) nanowire/nanobelt prepared in the example 2, and the analysis result is shown as B2 in the figure 1, so that the product has good crystallinity and obvious orientation; and the main phases of the samples are matched with the BiSe (PDF#29-0246), the strong diffraction peaks correspond to (005) crystal faces and (0012) crystal faces, and the purity of the synthesized product is high.
The bismuth selenide (BiSe) nanowire/nanoribbon prepared in example 2 was subjected to scanning electron microscope analysis, and the analysis result is shown in fig. 4, wherein the product length range is about 10-300 μm, as can be seen from fig. 4 (a), and the product is nanowire (b) and nanoribbon (c) with obvious one-dimensional characteristics, and the shape is regular, and Au particles are arranged at the top of the nanowire/nanoribbon, as can be seen from fig. 4 (b) and (c). Meanwhile, compared with the non-Au plating film, the quartz substrate treated by the Au plating film grows more and denser numbers of the BiSe nanowires/nanobelts.
The bismuth selenide (BiSe) nanowire/nanoribbon prepared in example 2 was subjected to electron microscope scanning and EDS (electron beam ionization) energy spectrum test, the test results are shown in fig. 6, fig. 6 shows EDS (electron beam ionization) energy spectrum images corresponding to the bismuth selenide (BiSe) nanowire/nanoribbon and the detected atomic ratio, and the result shows that the atomic ratio of Bi to Se is 49.26:50.74, and is close to the standard atomic ratio of BiSe of 1:1.
Comparative example 1
The preparation method is the same as in examples 1 and 2, except that: bi alone was used instead of the growth sources in examples 1 and 2, respectively 2 Se 3 The powder, no Bi powder, was used to set the control group for comparison, the other conditions were the same.
X-ray diffraction analysis was performed on the product prepared in comparative example 1, and the analysis result is shown in FIG. 2, wherein B1 is a product formed without Au plating treatment, and B2 is a product formed with Au plating treatment, and it can be seen that the main phase of the sample is equal to Bi 2 Se 3 (PDF#33-0214) and strong diffraction peaks correspond to (006) and (0015) crystal faces, and the result shows that the generated products are Bi 2 Se 3 Rather than BiSe.
Comparative example 2
The preparation method is the same as in example 1, except that: the distances from the quartz substrate to the heating center in example 1 were changed to 3 to 8cm and 15 to 20cm (3, 4, 5, 6, 7, 8cm and 15, 16, 17, 18, 19, 20cm, respectively) respectively, for comparison of the control group, and the other conditions were the same.
The result shows that almost no product is generated when the quartz substrate is 3cm to 8cm away from the heating center; when the distance from the heating center is 15 cm to 20cm, the shape of the product is in a block shape, and no nanowire/nanobelt is generated.
Comparative example 3
The preparation method is the same as in example 2, except that: the distances from the quartz substrate to the heating center in example 2 were changed to 3 to 8cm and 12 to 17cm (3, 4, 5, 6, 7, 8cm and 12, 13, 14, 15, 16, 17cm, respectively) respectively, for comparison of the control group, and the other conditions were the same.
The result shows that almost no product is generated when the quartz substrate is 3cm to 8cm away from the heating center; when the distance from the heating center is 12cm to 17cm, the generated product is changed into Bi 2 Se 3 。
Comparative example 4
The preparation method is the same as in examples 1 and 2, except that: the reaction temperatures in examples 1 and 2 were changed to 620, 630℃and 690, 700℃respectively, and were used for comparison in the control group, except that the conditions were the same.
The result shows that when the reaction temperature is 620-630 ℃, the growth effect is poor, and the product almost has no nanowires/nanobelts; when the reaction temperature is 690-700 ℃, the shape of the product is mostly tower-shaped and block-shaped with larger volume.
Comparative example 5
The preparation method is the same as in examples 1 and 2, except that: the air flow rates in examples 1 and 2 were changed to 50sccm, respectively, and the control group was set for comparison, and the other conditions were the same.
The results show that the growth effect is slightly different, but the product is still BiSe.
Comparative example 6
The preparation method is the same as in examples 1 and 2, except that: the air flow rates in examples 1 and 2 were changed to 100sccm, respectively, and the control group was set for comparison, with the same conditions.
The results show that the growth effect is slightly different, but the product is still BiSe.
Comparative example 7
The preparation method is the same as in examples 1 and 2, except that: the reaction times in examples 1 and 2 were changed to 30min, respectively, for comparison in the control group, and the other conditions were the same.
The results show that the growth effect is slightly different, but the product is still BiSe.
Comparative example 8
The preparation method is the same as in examples 1 and 2, except that: the reaction times in examples 1 and 2 were each changed to 6 hours for comparison in the control group, and the other conditions were the same.
The results show that the growth effect is slightly different, but the product is still BiSe.
In summary, the invention utilizes a simple chemical vapor deposition method by using Bi 2 Se 3 The powder and Bi powder are used as growth sources, quartz plates with/without Au plating films are used as growth substrates, under the condition of rare gas as carrier gas, bismuth selenide (BiSe) nanowires/nanobelts are prepared through reaction after being heated to a certain temperature, the prepared (BiSe) nanowires/nanobelts are regular in shape and have typical one-dimensional characteristics, the length of the nanowires/nanobelts is 10-300 mu m, the diameter is 200-800 nm, and the larger length-diameter ratio improves the physical properties of the nanowires/nanobelts, so that the application range of the bismuth selenide (BiSe) nanowires/nanobelts is expanded, and the application prospect is wide.
The embodiments of the present invention have been described in detail above, but the present invention is not limited to the described embodiments. It will be apparent to those skilled in the art that various changes, modifications, substitutions and alterations can be made to these embodiments without departing from the principles and spirit of the invention, and yet fall within the scope of the invention.
Claims (9)
1. A preparation method of bismuth selenide (BiSe) nanowires/nanobelts, which is characterized by comprising the following steps:
s1, bi 2 Se 3 Powder and Bi powder are used as growth sources, quartz plates with or without Au plating are used as growth substrates, and then Bi is used as a growth substrate 2 Se 3 Placing the powder in a heating center of a reaction area of the chemical vapor deposition equipment, placing Bi powder on the upstream of the heating center, and placing a quartz substrate on the downstream of the heating center;
s2, removing oxygen in the reaction area, inputting rare gas as carrier gas, maintaining the air pressure of the reaction area within a certain range, and heating to a certain temperature for reaction to prepare the bismuth selenide (BiSe) nanowire/nanobelt.
2. The method for preparing bismuth selenide (BiSe) nanowires/nanobelts according to claim 1, wherein in step S1, the Bi 2 Se 3 The mass ratio of the powder to the Bi powder is 1:1.
3. The method for preparing bismuth selenide (BiSe) nanowires/nanobelts according to claim 1, wherein in step S1, the Bi powder is 2-10 cm away from the heating center, the Au-free quartz substrate is 9-14 cm away from the heating center, and the Au-free quartz substrate is 9-11 cm away from the heating center.
4. The method for preparing bismuth selenide (BiSe) nanowires/nanobelts as claimed in claim 3, wherein the quartz substrate without Au plating is 9 to 12cm from the heating center, and the quartz substrate with Au plating is 9 to 10cm from the heating center.
5. The method for preparing bismuth selenide (BiSe) nanowires/nanobelts according to claim 1, wherein the reaction temperature is 640-680 ℃ and the reaction time is 0.5-6 h in the step S2.
6. The method for preparing bismuth selenide (BiSe) nanowires/nanobelts according to claim 5, wherein the reaction temperature is 640-680 ℃ for 1-2 h.
7. The method for preparing bismuth selenide (BiSe) nanowires/nanobelts according to claim 1, wherein in the step S2, the rare gas comprises Ar gas, and the gas flow is controlled to be 50-100 sccm.
8. The method for preparing bismuth selenide (BiSe) nanowires/nanobelts according to claim 1, wherein in step S2, the gas pressure of the reaction region is maintained below 150 Pa.
9. Bismuth selenide (BiSe) nanowires/nanobelts prepared by the preparation process of any one of claims 1 to 8.
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