CN110699754A - Magnetic topological insulator heterojunction single crystal material and synthetic method thereof - Google Patents
Magnetic topological insulator heterojunction single crystal material and synthetic method thereof Download PDFInfo
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- CN110699754A CN110699754A CN201911031909.2A CN201911031909A CN110699754A CN 110699754 A CN110699754 A CN 110699754A CN 201911031909 A CN201911031909 A CN 201911031909A CN 110699754 A CN110699754 A CN 110699754A
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- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
- C30B29/10—Inorganic compounds or compositions
- C30B29/46—Sulfur-, selenium- or tellurium-containing compounds
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- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B1/00—Single-crystal growth directly from the solid state
- C30B1/10—Single-crystal growth directly from the solid state by solid state reactions or multi-phase diffusion
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Abstract
The invention provides a magnetic topological insulator heterojunction single crystal material and a synthetic method thereof, wherein the synthetic method comprises the following steps: grinding metal and chalcogen, and filling the ground metal and chalcogen into a quartz tube for vacuum tube sealing; heating and preserving heat of the sealed quartz tube, and then cooling; cooling the cooled quartz tube again; and performing ice-bath quenching on the quartz tube after being cooled again to obtain the heterojunction single crystal material of the magnetic topological insulator. The method has the advantages of simple operation, no need of any transfer method, no need of expensive special production equipment, higher production efficiency and capability of quickly preparing the heterojunction single crystal material with the natural magnetic topological insulator.
Description
Technical Field
The invention belongs to the technical field of topological insulator heterojunction materials, and particularly relates to a magnetic topological insulator heterojunction single crystal material and a synthetic method thereof.
Background
The importance of the anomalous quantum hall effect is that in the absence of any external magnetic field, human beings can develop a new generation of low-energy consumption transistors and electronic devices by using the non-dissipative edge states, so as to solve the bottleneck problems of computer heating and moore's law, and therefore the research result will promote the development of the new generation of low-energy consumption transistors and electronic devices. However, the abnormal quantum hall effect is extremely demanding on the material.
And ferromagnetism is introduced into a topological insulator, and the defect of time symmetry of the ferromagnetism can realize the abnormal quantum Hall effect. Two methods are currently commonly used to introduce ferromagnetism in topological insulators. One is doping the magnetic material in the topological insulator and the other is by making the ferromagnetic and topological insulator heterojunction interface. However, these methods are complicated to operate, require expensive special production equipment, and have high production cost, long production period and low production efficiency.
Disclosure of Invention
Aiming at the problems in the prior art, the invention provides a magnetic topological insulator heterojunction single crystal material and a synthesis method thereof, which have the advantages of simple operation, no need of any transfer method, no need of expensive special production equipment, higher production efficiency and capability of quickly preparing the natural magnetic topological insulator heterojunction single crystal material.
In order to achieve the purpose, the technical scheme adopted by the invention for solving the technical problems is as follows: a synthetic method of a magnetic topological insulator heterojunction single crystal material comprises the following steps:
(1) grinding the metal, and then putting the metal into a quartz tube for vacuum tube sealing;
(2) heating the quartz tube sealed in the step (1) to 900-1100 ℃, preserving heat for 2-4 hours, and then cooling to 600-700 ℃;
(3) reducing the temperature of the quartz tube cooled in the step (2) to 500-590 ℃ at a cooling rate of 1-3 ℃/d for 6-8 d;
(4) and (4) performing ice bath quenching on the quartz tube cooled again in the step (3) to obtain the magnetic topological insulator heterojunction single crystal material MBT.
Further, in the step (1), the metal is transition metal or rare earth metal, including manganese, bismuth or antimony, and the chalcogen element is tellurium, selenium or sulfur, and the molar ratio of the chalcogen element to the tellurium, selenium or sulfur is 1: 3-5: 5-10.
Further, the molar ratio is 1: 2-4: 4-10.
Further, when the temperature is reduced in the step (2), the temperature reduction rate is 30-50 ℃/h, and the temperature is reduced for 9-11 h.
Further, the cooling rate in the step (2) is 40 ℃/h.
Further, the cooling rate in the step (3) is 2 ℃/d.
Further, M is a transition metal or a rare earth metal, B is bismuth or antimony, and T is tellurium, selenium or sulfur.
The magnetic topological insulator heterojunction single crystal material is prepared by adopting the synthesis method of the magnetic topological insulator heterojunction single crystal material.
Wherein the single crystal material has a composition of (MB)2T4)m(B2T3) n, wherein m is 1 to 5 and n is 1 to 5.
In summary, the invention has the following advantages:
1. compared with the traditional method for preparing the thin film heterojunction, the preparation method is simple, the preparation of the natural heterojunction magnetic topological insulator single crystal material can be realized only by heating the quartz tube by the tube furnace and controlling the temperature of each reaction process, expensive production equipment is not needed, the production cost can be effectively reduced, the magnetic topological insulator single crystal material with the natural heterojunction is prepared, the appearance of the obtained single crystal material is relatively easy to control, and the obtained single crystal material has better stability.
2. Compared with the complex operation of the traditional method for preparing the two-dimensional film heterojunction by the transfer method, the method is simple and convenient to operate, and the heterojunction single crystal MBT with the natural magnetic topological insulator can be obtained only by proportioning manganese, bismuth and tellurium, placing the mixture in a high-temperature furnace for heating and heat preservation, carrying out cooling treatment twice and carrying out quenching treatment.
Drawings
FIG. 1 is a schematic diagram showing characterization results of an X-ray single crystal diffraction instrument;
FIG. 2 is a diagram showing the characterization results of a magnetic measurement system;
FIG. 3 is a diagram showing the characterization results of the magnetic measurement system.
Detailed Description
Example 1
A synthetic method of a magnetic topological insulator heterojunction single crystal material comprises the following steps:
(1) grinding manganese, bismuth and tellurium, and then filling the ground materials into a quartz tube for vacuum tube sealing; wherein the molar ratio of manganese to bismuth to tellurium is 1:2: 4;
(2) heating the quartz tube sealed in the step (1) to 900 ℃, preserving heat for 2h, then cooling at a cooling rate of 30 ℃/h for 10h, and cooling to 600 ℃;
(3) reducing the temperature of the quartz tube cooled in the step (2) to 584 ℃ at a cooling rate of 2 ℃/d for 8 d;
(4) and (4) performing ice bath quenching on the quartz tube cooled again in the step (3) to obtain the magnetic topological insulator heterojunction single crystal material MBT.
Example 2
A synthetic method of a magnetic topological insulator heterojunction single crystal material comprises the following steps:
(1) grinding manganese, bismuth and tellurium, and then filling the ground materials into a quartz tube for vacuum tube sealing; wherein the molar ratio of manganese to bismuth to tellurium is 1:4: 7;
(2) heating the quartz tube sealed in the step (1) to 1000 ℃, preserving heat for 3h, then cooling at a cooling rate of 40 ℃/h for 10h, and cooling to 600 ℃;
(3) reducing the temperature of the quartz tube cooled in the step (2) to 586 ℃ at a cooling rate of 2 ℃/d for 7 d;
(4) and (4) performing ice bath quenching on the quartz tube cooled again in the step (3) to obtain the magnetic topological insulator heterojunction single crystal material MBT.
Example 3
A synthetic method of a magnetic topological insulator heterojunction single crystal material comprises the following steps:
(1) grinding manganese, antimony and selenium, and then filling the ground materials into a quartz tube for vacuum tube sealing; wherein the molar ratio of manganese to antimony to selenium is 1:5: 9;
(2) heating the quartz tube sealed in the step (1) to 1100 ℃, preserving the heat for 4h, then cooling for 10h at the cooling rate of 50 ℃/h, and cooling to 600 ℃;
(3) reducing the temperature of the quartz tube cooled in the step (2) to 576 ℃ at a cooling rate of 3 ℃/d for 8 d;
(4) and (4) performing ice bath quenching on the quartz tube cooled again in the step (3) to obtain the magnetic topological insulator heterojunction single crystal material MBT.
Example 4
A synthetic method of a magnetic topological insulator heterojunction single crystal material comprises the following steps:
(1) grinding manganese, antimony and sulfur, and then filling the ground manganese, antimony and sulfur into a quartz tube for vacuum tube sealing; wherein the molar ratio of manganese to antimony to sulfur is 1:4: 7;
(2) heating the quartz tube sealed in the step (1) to 1000 ℃, preserving heat for 3h, then cooling at a cooling rate of 40 ℃/h for 10h, and cooling to 600 ℃;
(3) reducing the temperature of the quartz tube cooled in the step (2) to 586 ℃ at a cooling rate of 2 ℃/d for 7 d;
(4) and (4) performing ice bath quenching on the quartz tube cooled again in the step (3) to obtain the magnetic topological insulator heterojunction single crystal material MBT.
The magnetic topological insulator material MBT with the natural heterojunction obtained in the examples 1-4 is characterized by an X-ray powder diffractometer and a magnetic measurement system MPMS3, and the results are shown in the figures 1-3. As can be seen from FIGS. 1 to 3, the magnetic topological insulator heterojunction single crystal material prepared by the method has high quality, obvious magnetic susceptibility and magnetization intensity, and antiferromagnetic transition transformation occurs when the magnetic field intensity reaches 17T.
Comparative example
A preparation method of a heterojunction with graphene and europium sulfide comprises the following steps: synthesizing single-layer graphene by chemical vapor deposition, and transferring the graphene onto a silicon dioxide substrate by utilizing the adhesion of dimethyl siloxane; then annealing for 3 hours at the temperature of 170-200 ℃ to remove the residual glue on the surface of the graphene; and finally depositing europium sulfide on the graphene at room temperature to obtain the material.
In the preparation process of the method provided by the comparative example, the graphene needs to be transferred to the silicon dioxide substrate, the transfer operation process is complex, glue residues are easy to exist on the surface of the graphene during annealing, special production equipment is needed, and the production cost is high. The synthesis method provided by the invention does not relate to any transfer method, only needs a tube furnace for heating, does not need special equipment, is simple and quick to operate, improves the synthesis efficiency, and obtains the single crystal material with a natural heterojunction structure.
While the present invention has been described in detail with reference to the illustrated embodiments, it should not be construed as limited to the scope of the present patent. Various modifications and changes may be made by those skilled in the art without inventive step within the scope of the appended claims.
Claims (8)
1. A synthetic method of a magnetic topological insulator heterojunction single crystal material is characterized by comprising the following steps:
(1) grinding metal and chalcogen, and filling the ground metal and chalcogen into a quartz tube for vacuum tube sealing;
(2) heating the quartz tube sealed in the step (1) to 900-1100 ℃, preserving heat for 2-4 hours, and then cooling to 600-700 ℃;
(3) reducing the temperature of the quartz tube cooled in the step (2) to 500-590 ℃ at a cooling rate of 1-3 ℃/d for 6-8 d;
(4) and (4) performing ice bath quenching on the quartz tube cooled again in the step (3) to obtain the magnetic topological insulator heterojunction single crystal material MBT.
2. The method for synthesizing the magnetic topological insulator heterojunction single crystal material as claimed in claim 1, wherein the metal in the step (1) is a transition metal or a rare earth metal, including manganese, bismuth or antimony, and the chalcogen element is tellurium, selenium or sulfur, and the molar ratio of the chalcogen element to the sulfur is 1: 3-5: 5-10.
3. The method for synthesizing the magnetic topological insulator heterojunction single crystal material as claimed in claim 2, wherein the molar ratio is 1:2 to 4:4 to 10.
4. The method for synthesizing the magnetic topological insulator heterojunction single crystal material as claimed in claim 1, wherein the cooling rate in the step (2) is 30-50 ℃/h and the cooling rate is 9-11 h.
5. The method for synthesizing the magnetic topological insulator heterojunction single crystal material as claimed in claim 4, wherein the cooling rate in the step (2) is 40 ℃/hr.
6. The method for synthesizing the magnetic topological insulator heterojunction single crystal material as claimed in claim 1, wherein the cooling rate in the step (3) is 2 ℃/d.
7. The method for synthesizing the magnetic topological insulator heterojunction single crystal material as claimed in claim 1, wherein M is a transition metal or a rare earth metal, B is bismuth or antimony, and T is tellurium, selenium or sulfur.
8. The magnetic topological insulator heterojunction single-crystal material prepared by adopting the synthesis method of the magnetic topological insulator heterojunction single-crystal material as claimed in any one of claims 1 to 7.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112002766A (en) * | 2020-08-28 | 2020-11-27 | 河南师范大学 | Based on MnBi2Te4Single-layer nanoscale PN junction diode rectifier |
| CN114561687A (en) * | 2022-02-28 | 2022-05-31 | 福建师范大学 | S-doped MnBi2Te4Method for producing single crystal |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103526297A (en) * | 2013-10-17 | 2014-01-22 | 西南交通大学 | Method for preparing topological insulator Bi2Se3 film |
| CN108428789A (en) * | 2018-02-05 | 2018-08-21 | 清华大学 | Multichannel topological insulator structure, preparation method and electricity device |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103526297A (en) * | 2013-10-17 | 2014-01-22 | 西南交通大学 | Method for preparing topological insulator Bi2Se3 film |
| CN108428789A (en) * | 2018-02-05 | 2018-08-21 | 清华大学 | Multichannel topological insulator structure, preparation method and electricity device |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112002766A (en) * | 2020-08-28 | 2020-11-27 | 河南师范大学 | Based on MnBi2Te4Single-layer nanoscale PN junction diode rectifier |
| CN112002766B (en) * | 2020-08-28 | 2023-07-25 | 河南师范大学 | MnBi-based alloy 2 Te 4 Single-layer nano-scale PN junction diode rectifier |
| CN114561687A (en) * | 2022-02-28 | 2022-05-31 | 福建师范大学 | S-doped MnBi2Te4Method for producing single crystal |
| CN114561687B (en) * | 2022-02-28 | 2023-11-17 | 福建师范大学 | S-doped MnBi 2 Te 4 Method for producing single crystal |
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