CN117187956A - Large band gap topological insulator material Bi 4 Br 4 Nanostructure and method for preparing same - Google Patents
Large band gap topological insulator material Bi 4 Br 4 Nanostructure and method for preparing same Download PDFInfo
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Abstract
The invention relates to a large band gap topological insulator material Bi 4 Br 4 A nano structure and a preparation method thereof belong to the technical field of crystal materials. The nanostructure is prepared by a physical vapor transport method, and the method adopts Bi 4 Br 4 The monocrystal is used as a raw material, and Bi with a two-dimensional high-quality nano structure is directly prepared on a silicon wafer substrate with an Au film plated on the surface by heating the raw material end in vacuum at 320-400 ℃ and keeping the temperature for 30-90 min 4 Br 4 . The Bi is 4 Br 4 The nano structure has uniform phase and low impurity content.
Description
Technical Field
The invention relates to a large band gap topological insulator material Bi 4 Br 4 A nano structure and a preparation method thereof belong to the technical field of crystal materials.
Background
Topological insulator is a novel quantum state, in short, has a similar bulk band gap as a common insulator in the body, but shows a conductive channel without a band gap on the surface, and shows a linear energy-momentum dispersion relation, spin and momentum locking of surface state electrons and is protected by time reversal symmetry. And the three-dimensional material with the surface state or the two-dimensional material with the edge state is more stable than the common metal and is not influenced by defects or impurity scattering, so that the topological insulator is considered to have great application potential in the fields of low-power transmission, sensing, quantum detection and the like.
Bi 4 Br 4 Is predicted to be a large bandgap topological insulator with its nanostructure having Shan Di rad cone edge states spanning the bulk bandgap, an ideal carrier for non-dissipative transport. However, current research is mainly focused on three-dimensional materials, and as research goes deep, it is found that it is difficult to directly peel single-layer or few-layer structural materials from the three-dimensional materials, so that subsequent device research and future application of the materials are greatly hindered. Therefore, bi with high-quality nano structure in two-dimensional state is directly prepared 4 Br 4 Is particularly important.
Chinese patent CN113445124B discloses a Bi 4 Br 4 The method adopts a molecular beam epitaxial growth technology to grow a Bi film on a substrate; the substrate is a cleavage plane of a transition metal chalcogenide single crystal (001) or an HOPG (0001); biBr is prepared 3 Depositing Bi and Br on the surface of the Bi film by adopting a high-temperature cracking mode, and ending the deposition when the thickness of the film deposited on the surface of the Bi film is 4-5 times that of the Bi film; when the substrate is a cleavage plane of HOPG (0001), the thin film on the substrate is Bi 4 Br 4 A film;when the substrate is a transition metal chalcogenide monocrystal (0001) surface, the film on the substrate is a BiBr film, and annealing to obtain Bi 4 Br 4 A film. The method has complex process and high energy consumption, and can not realize Bi 4 Br 4 The regulation of the nano structure and the uniform nano material is difficult to obtain.
Disclosure of Invention
In view of the above, the present invention aims to provide a large band gap topology insulator material Bi 4 B r4 Nano structure and preparation method thereof, wherein the nano structure is prepared from Bi 4 Br 4 The monocrystal is raw material, the silicon chip is substrate, and the monocrystal is directly grown on the substrate by a brand new physical vapor transport method, which is specific to Bi 4 Br 4 Subsequent device research and future applications are of great value.
In order to achieve the above object, the technical scheme of the present invention is as follows.
Large band gap topological insulator material Bi 4 Br 4 The preparation method of the nanostructure comprises the following steps:
(1) The Bi is treated under the environment that the water and oxygen content is less than 0.1ppm 4 Br 4 The monocrystal and the silicon chip are respectively placed at two ends of a quartz tube, and the quartz tube is vacuum sealed, and the vacuum degree is less than or equal to 1 multiplied by 10 -4 Pa；
(2) Taking the end of the quartz tube sealed in the step (1) where the silicon chip is placed as a growth end, and placing Bi 4 Br 4 One end of the single crystal is taken as a raw material end, the raw material end is heated to 320-400 ℃ from room temperature, the temperature is kept for 30-100 min, then the temperature is reduced to room temperature, and the growth end is not heated;
(3) Opening a quartz tube, and generating a large band gap topological insulator material Bi on the surface of the silicon wafer 4 Br 4 A nanostructure.
Preferably, in the step (1), the surface of the silicon wafer is uniformly plated with an Au film with the thickness of 10-20 nm. The gold film may regulate the type of nanostructure, e.g., the thicker the gold film, the more prone the nanostructure to thin film structures.
Preferably, in step (1), the sealed quartzIn the tube, the vacuum degree is less than or equal to 1X 10 -4 Pa。
Preferably, in the step (2), the quartz tube sealed in the step (1) is placed in a double-temperature-zone tube furnace, the raw material end is placed at the high-temperature end of the double-temperature-zone tube furnace, and the growth end is placed at the low-temperature end of the double-temperature-zone tube furnace. Although the low temperature end does not start heating, the low temperature end also has temperature change due to heat conduction of the temperature of the high temperature end, and the high temperature end and the low temperature end of the double-temperature-zone tube furnace are both provided with thermocouples, so that the temperature indication of the low temperature end can be directly displayed, and the actual working condition of the low temperature end can be conveniently observed and recorded.
Preferably, in the step (2), when the temperature of the raw material end is 350-365 ℃ and the constant temperature holding time is 30-40 min, the Bi is prepared 4 Br 4 The content of the nano wires in the nano structure is more than 70%, and the rest is nano sheets; when the temperature of the raw material end is 365-385 ℃, and the constant temperature holding time is prolonged to 60-80 min, the Bi is prepared 4 Br 4 The content of the nanosheets in the nano structure is more than 70%, and the balance is nanowires; when the temperature of the raw material end is 385-400 ℃ and the constant temperature holding time is prolonged to 90-100 min, the Bi is prepared 4 Br 4 The content of the nano film in the nano structure is more than 70%, and the rest is nano sheet.
Preferably, in the step (2), the temperature rising and falling rate is 4 ℃/min to 5 ℃/min.
Large band gap topological insulator material Bi 4 Br 4 A nanostructure comprising one or more of a nanoplatelet, a nanofilm, and a nanowire.
Advantageous effects
1. The invention provides a large band gap topological insulator material Bi 4 Br 4 A nanostructure comprising at least one of a nanoplatelet, a nanoribbon, and a nanofilm; the Bi is 4 Br 4 The nano structure has uniform phase and low impurity content, can be directly transferred to manufacture devices, and has great potential application value in the field of low-power-consumption devices.
2. The invention provides a large band gap topological insulator material Bi 4 Br 4 Nano-structure, provided withThe nanostructure is prepared by a physical vapor transport method, and the method uses Bi 4 Br 4 The monocrystal is used as a raw material, and Bi with a two-dimensional high-quality nano structure is directly prepared on a silicon wafer substrate by vacuum heating the raw material end at 320-400 ℃ and keeping the temperature for 30-90 min 4 Br 4 The method comprises the steps of carrying out a first treatment on the surface of the The Bi4Br can be realized by controlling the heating temperature and the constant temperature maintenance of the raw material end in physical vapor transport 4 Adjustment of the nanostructure. It has Bi more than the material prepared by the flux method 4 Br 4 The intrinsic properties of the material provide a material basis for studying its properties. The method has simple process and strong practicability, and can be applied to the preparation of the nano structure of other materials.
Drawings
FIG. 1 shows Bi as described in the embodiment of the present invention 4 Br 4 X-ray diffraction (XRD) pattern of single crystals.
FIG. 2 shows Bi as described in example 1 4 Br 4 Scanning Electron Microscope (SEM) images of the material.
FIG. 3 shows Bi as described in example 1 4 Br 4 XRD pattern of the material.
FIG. 4 is a diagram of Bi as described in example 2 4 Br 4 SEM image of the material.
FIG. 5 shows Bi as described in example 4 4 Br 4 SEM image of the material.
FIG. 6 shows Bi as described in example 1, example 2 and example 4 4 Br 4 Material X-ray spectroscopy (EDS) map.
Detailed Description
The present invention will be described in further detail with reference to specific examples.
The reagents and apparatus used in the examples below are all conventional in the art and are commercially available.
In the following examples 1 to 4: bi is used 4 Br 4 The monocrystal is prepared by adopting a fluxing agent method, and the specific steps are as follows:
(1) Packaging Bi particles in a quartz tube filled with hydrogen gas at 0.8 atm, and annealing the Bi particles at 220K to remove an oxide layer on the surface;
bi is used as fluxing agent, biBr 3 As raw material, biBr in stoichiometric ratio 3 Bi=1:16, raw materials and fluxing agents are weighed into a quartz tube, the mass of the raw materials is 7.5g, the weighing error is 0.1%, quartz cotton is added, and then the quartz tube is subjected to vacuum degree of 1 multiplied by 10 -4 Sealing in a pipe sealing system of Pa;
the fluxing agent Bi and the raw material BiBr 3 The purity of (2) is 99.99%;
(2) Placing the vacuum sealed quartz tube in the step (1) in a muffle furnace, heating to 500 ℃ for 3 hours, maintaining at 500 ℃ for 10 hours, then cooling to 310 ℃ for 15 hours, maintaining at the temperature for 5 hours, finally reducing to 278 ℃ at the speed of 1 ℃/h, centrifuging at 278 ℃, and adsorbing excessive Bi by quartz wool in the centrifuging process, and separating the Bi from single crystals; the quartz tube was opened to give the product.
The structure of the obtained product was analyzed by X-ray diffraction (XRD) and as shown in FIG. 1, it was confirmed that the product was Bi by comparison with a standard card (ICSD number: 98-000-1560) 4 Br 4 And (3) single crystals.
In the following examples 1 to 4: the length of the silicon wafer is 4-5 cm, the width of the silicon wafer is 6-7 mm, and the silicon wafer is uniformly electroplated with an Au film with the thickness of 10-20 nm; the quartz tube used had an inner diameter of 8mm and an outer diameter of 12mm.
Example 1
Large band gap topological insulator material Bi 4 Br 4 A nanostructure, the nanostructure being predominantly a nanoplatelet; the method is prepared by adopting a physical gas phase transportation method and comprises the following specific steps:
(1) Weighing 0.02g Bi in a glove box with water and oxygen content less than 0.1ppm and argon atmosphere 4 Br 4 The single crystal and the silicon wafer with the Au film uniformly plated on the surface are respectively placed at two ends of a quartz tube, the vacuum tube sealing system is used for carrying out gas washing treatment by argon, after the gas washing is finished, a mechanical pump is used for evacuating the argon in the tube, and the quartz tube is subjected to vacuum degree of 1 multiplied by 10 -4 Sealing in a pipe sealing system of Pa;
(2) Placing the quartz tube sealed in the step (1) in a double-temperature-zone tube furnace with a temperature zone of 10cmIn which Bi is placed in a quartz tube 4 Br 4 The method comprises the steps that one end of a single crystal is used as a raw material end, one end for placing a silicon wafer is used as a growing end, the raw material end is placed at a high-temperature end of a double-temperature tube furnace, the growing end is placed at a low-temperature end of the double-temperature tube furnace, the high-temperature end is heated from room temperature to 320 ℃ for 80 minutes, the temperature is kept at 320 ℃ for 90 minutes, the growing end is not heated, then the temperature is reduced to room temperature for 80 minutes, and the tube furnace is closed;
(3) Opening the quartz tube, and generating a large band gap topological insulator material Bi on the surface of the silicon wafer 4 Br 4 。
After the quartz tube is opened, the surface of the silicon wafer can be obviously blackened by naked eyes; the silicon wafer surface of example 1 was observed by Scanning Electron Microscope (SEM) to generate Bi 4 Br 4 Morphology of the material, the result is shown in FIG. 2, the Bi 4 Br 4 The material is mainly in the shape of a sheet, the length and the width of the nano sheet are in the micrometer scale, the thickness is in the nanometer scale, and the Bi is prepared 4 Br 4 In the nano structure, the content of the nano sheet is more than 70 percent.
Determination of Bi prepared in example 1 by X-ray energy Spectrometry (EDS) analysis 4 Br 4 The elemental ratios of the materials, as shown in FIG. 6 (a), resulted in the appearance of characteristic peaks of Bi and Br, with the ratio of the components of each element approaching 1:1, while the EDS results between the selected regions differ little, indicating that Bi is present 4 Br 4 The material has high purity and good uniformity.
Determination of Bi prepared in example 1 by X-ray diffraction analysis (XRD) 4 Br 4 As shown in FIG. 3, the structure of the material is compared with that of a standard card (ICSD number: 98-000-1560), and Bi obtained in example 1 4 Br 4 Each spectrum peak of the material is close to Bi 4 Br 4 Single crystal diffraction peak in which the peak around 2θ=70° is derived from the substrate, illustrating Bi prepared in example 1 4 Br 4 The material is of a single crystal structure.
Example 2
Large band gap topological insulator material Bi 4 Br 4 A nanostructure, the nanostructure being predominantly a nanofilm; by physical vapor transportThe preparation method comprises the following specific steps:
(1) Weighing 0.02g Bi in a glove box with water and oxygen content less than 0.1ppm and argon atmosphere 4 Br 4 The single crystal and the silicon wafer with the Au film uniformly plated on the surface are respectively placed at two ends of a quartz tube, the vacuum tube sealing system is used for carrying out gas washing treatment by argon, after the gas washing is finished, a mechanical pump is used for evacuating the argon in the tube, and the quartz tube is subjected to vacuum degree of 1 multiplied by 10 -4 Sealing in a pipe sealing system of Pa;
(2) Placing the quartz tube sealed in the step (1) in a double-temperature-zone tube furnace with a temperature zone of 10cm, and placing Bi in the quartz tube 4 Br 4 The method comprises the steps that one end of a single crystal is used as a raw material end, one end for placing a silicon wafer is used as a growing end, the raw material end is placed at a high-temperature end of a double-temperature tube furnace, the growing end is placed at a low-temperature end of the double-temperature tube furnace, the high-temperature end is heated from room temperature to 320 ℃ for 80 minutes, the temperature is kept at 320 ℃ for 60 minutes, the growing end is not heated, then the temperature is reduced to room temperature for 80 minutes, and the tube furnace is closed;
(3) Opening the quartz tube, and generating a large band gap topological insulator material Bi on the surface of the silicon wafer 4 Br 4 。
After the quartz tube is opened, the surface of the silicon wafer can be obviously blackened by naked eyes; observation of example 2 silicon wafer surface to generate Bi by Scanning Electron Microscope (SEM) 4 Br 4 The morphology of the material, the result is shown in FIG. 4, the Bi 4 Br 4 The material is mainly a nano film, and grows on a silicon wafer plated with an Au film; bi prepared 4 Br 4 In the nanostructure, the content of the nano film is more than 70%.
Determination of Bi prepared in example 2 by X-ray energy Spectrometry (EDS) analysis 4 Br 4 The elemental ratios of the materials, as shown in FIG. 6 (b), resulted in the appearance of characteristic peaks of Bi and Br, with the ratio of the components of each element approaching 1:1, while the EDS results between the selected regions differ little, indicating that Bi is present 4 Br 4 The material has high purity and good uniformity.
Determination of Bi prepared in example 2 by X-ray diffraction analysis (XRD) 4 Br 4 The structure of the material and the results show thatBi prepared in example 2 4 Br 4 The material is in a polycrystalline structure.
Compared with the CN113445124B film, the film prepared by the embodiment is denser, the used equipment is simple and easy to operate, and the price cost is lower.
Example 3
Large band gap topological insulator material Bi 4 Br 4 A nanostructure, the nanostructure being predominantly a nanofilm; the method is prepared by adopting a physical gas phase transportation method and comprises the following specific steps:
(1) Weighing 0.02g Bi in a glove box with water and oxygen content less than 0.1ppm and argon atmosphere 4 Br 4 The single crystal and the silicon wafer with the Au film uniformly plated on the surface are respectively placed at two ends of a quartz tube, the vacuum tube sealing system is used for carrying out gas washing treatment by argon, after the gas washing is finished, a mechanical pump is used for evacuating the argon in the tube, and the quartz tube is subjected to vacuum degree of 1 multiplied by 10 -4 Sealing in a pipe sealing system of Pa;
(2) Placing the quartz tube sealed in the step (1) in a double-temperature-zone tube furnace with a temperature zone of 10cm, and placing Bi in the quartz tube 4 Br 4 One end of the single crystal is a raw material end, one end for placing a silicon wafer is a growth end, the raw material end is placed at a high-temperature end of a double-temperature tube furnace, the growth end is placed at a low-temperature end of the double-temperature tube furnace, the high-temperature end is heated from room temperature to 400 ℃ for 80 minutes, the temperature is kept at the 400 ℃ for 60 minutes, the growth end is not heated, then the temperature is reduced to room temperature for 80 minutes, and the tube furnace is closed;
(3) Opening the quartz tube, and generating a large band gap topological insulator material Bi on the surface of the silicon wafer 4 Br 4 。
After the quartz tube is opened, the surface of the silicon wafer can be obviously blackened by naked eyes; scanning Electron Microscope (SEM) observation of the surface of the silicon wafer of example 3 to produce Bi 4 Br 4 Morphology of the material, results similar to example 2, bi 4 Br 4 The material is mainly a nano film and grows on a silicon wafer plated with an Au film; bi prepared 4 Br 4 In the nanostructure, the content of the nano film is more than 70%.
Determination of reality using X-ray energy spectrum (EDS) analysisBi prepared in example 3 4 Br 4 The elemental ratios of the materials, resulting in the appearance of characteristic peaks of Bi and Br similar to example 2, with a ratio of the components of each element close to 1:1, with minimal EDS differences between the selected regions, indicating that Bi is present 4 Br 4 The material has high purity and good uniformity.
Determination of Bi prepared in example 3 by X-ray diffraction analysis (XRD) 4 Br 4 The structure of the material and the results are similar to those of example 2, illustrating Bi prepared in example 3 4 Br 4 The material is in a polycrystalline structure.
Example 4
Large band gap topological insulator material Bi 4 Br 4 A nanostructure, the nanostructure being predominantly a nanowire; the method is prepared by adopting a physical gas phase transportation method and comprises the following specific steps:
(1) Weighing 0.02g Bi in a glove box with water and oxygen content less than 0.1ppm and argon atmosphere 4 Br 4 The single crystal and the silicon wafer with the Au film uniformly plated on the surface are respectively placed at two ends of a quartz tube, the vacuum tube sealing system is used for carrying out gas washing treatment by argon, after the gas washing is finished, a mechanical pump is used for evacuating the argon in the tube, and the quartz tube is subjected to vacuum degree of 1 multiplied by 10 -4 Sealing in a pipe sealing system of Pa;
(2) Placing the quartz tube sealed in the step (1) in a double-temperature-zone tube furnace with a temperature zone of 10cm, and placing Bi in the quartz tube 4 Br 4 One end of the single crystal is a raw material end, one end for placing a silicon wafer is a growth end, the raw material end is placed at a high-temperature end of a double-temperature tube furnace, the growth end is placed at a low-temperature end of the double-temperature tube furnace, the high-temperature end is heated from room temperature to 400 ℃ for 80min, the temperature is kept at the 400 ℃ for 30min, the growth end is not heated, then the temperature is reduced to room temperature for 80min, and the tube furnace is closed;
(3) Opening the quartz tube, and generating a large band gap topological insulator material Bi on the surface of the silicon wafer 4 Br 4 。
After the quartz tube is opened, the surface of the silicon wafer can be obviously blackened by naked eyes; the surface of the silicon wafer of example 4 was observed by a Scanning Electron Microscope (SEM) to produce Bi 4 Br 4 MaterialThe morphology of (2) is shown in FIG. 5, and the Bi 4 Br 4 The material is mainly in a strip shape; bi prepared 4 Br 4 In the nano structure, the content of the nano wires is more than 70 percent.
Determination of Bi prepared in example 4 by X-ray energy Spectrometry (EDS) analysis 4 Br 4 The elemental ratios of the materials, as shown in FIG. 6 (c), resulted in the appearance of characteristic peaks of Bi and Br, with the ratio of the components of each element approaching 1:1, while the EDS results between the selected regions differ little, indicating that Bi is present 4 Br 4 The material has high purity and good uniformity.
Determination of Bi prepared in example 4 by X-ray diffraction analysis (XRD) 4 Br 4 The structure of the material, the result being similar to example 1, illustrates Bi prepared in example 4 4 Br 4 The material is of a single crystal structure.
In view of the foregoing, it will be appreciated that the invention includes but is not limited to the foregoing embodiments, any equivalent or partial modification made within the spirit and principles of the invention.
Claims (7)
1. Large band gap topological insulator material Bi 4 Br 4 The preparation method of the nanostructure is characterized by comprising the following steps: the method comprises the following steps:
(1) The Bi is treated under the environment that the water and oxygen content is less than 0.1ppm 4 Br 4 The monocrystal and the silicon chip are respectively placed at two ends of the quartz tube, and the quartz tube is vacuum sealed;
(2) Taking the end of the quartz tube sealed in the step (1) where the silicon chip is placed as a growth end, and placing Bi 4 Br 4 One end of the single crystal is taken as a raw material end, the raw material end is heated to 320-400 ℃ from room temperature, the temperature is kept for 30-100 min, then the temperature is reduced to room temperature, and the growth end is not heated;
(3) Opening a quartz tube, and generating a large band gap topological insulator material Bi on the surface of the silicon wafer 4 Br 4 A nanostructure.
2. The method as claimed in claim 1Is a large band gap topological insulator material Bi 4 Br 4 The preparation method of the nanostructure is characterized by comprising the following steps: in the step (1), the vacuum degree in the sealed quartz tube is less than or equal to 1 multiplied by 10 -4 Pa。
3. A large band gap topology insulator material Bi as recited in claim 1 4 Br 4 The preparation method of the nanostructure is characterized by comprising the following steps: in the step (1), the surface of the silicon wafer is uniformly plated with an Au film with the thickness of 10-20 nm.
4. A large band gap topology insulator material Bi as recited in claim 1 4 Br 4 The preparation method of the nanostructure is characterized by comprising the following steps: in the step (2), the quartz tube sealed in the step (1) is placed in a double-temperature-zone tube furnace, the raw material end is placed at the high-temperature end of the double-temperature-zone tube furnace, and the growth end is placed at the low-temperature end of the double-temperature-zone tube furnace.
5. A large band gap topology insulator material Bi as recited in claim 1 4 Br 4 The preparation method of the nanostructure is characterized by comprising the following steps: in the step (2), when the temperature of the raw material end is 350-365 ℃ and the constant temperature holding time is 30-40 min, the Bi is prepared 4 Br 4 The content of the nano wires in the nano structure is more than 70%, and the rest is nano sheets; when the temperature of the raw material end is 365-385 ℃, and the constant temperature holding time is prolonged to 60-80 min, the Bi is prepared 4 Br 4 The content of the nanosheets in the nano structure is more than 70%, and the balance is nanowires; when the temperature of the raw material end is 385-400 ℃ and the constant temperature holding time is prolonged to 90-100 min, the Bi is prepared 4 Br 4 The content of the nano film in the nano structure is more than 70%, and the rest is nano sheet.
6. A large band gap topology insulator material Bi as recited in claim 1 4 Br 4 The preparation method of the nanostructure is characterized by comprising the following steps: in the step (2), the temperature rising and falling rate is 4-5 ℃/min.
7. Large band gap topological insulator material Bi 4 Br 4 The nanostructure is characterized in that: the method of any one of claims 1-6, wherein the nanostructure comprises one or more of a nanosheet, a nanofilm, and a nanowire.
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