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CN-121990527-A - Ternary layered selenide Ge0.85Bi2.15+xSe4Semiconductor material and preparation method thereof

CN121990527ACN 121990527 ACN121990527 ACN 121990527ACN-121990527-A

Abstract

The invention relates to the technical field of crystal material preparation, in particular to a ternary layered selenide Ge 0.85 Bi 2.15+x Se 4 semiconductor material and a preparation method thereof. The preparation method comprises the steps of weighing germanium powder, bismuth powder and selenium powder according to a molar ratio in a chemical formula Ge 0.85 Bi 2.15+x Se 4 , wherein x is more than or equal to 0 and less than or equal to 0.06, uniformly mixing the weighed raw materials, placing the raw materials into a quartz tube, vacuumizing, sealing the quartz tube, placing the vacuum-sealed quartz tube into a heating furnace, heating the quartz tube to 900-950 ℃ from room temperature, preserving the temperature for 12-24 hours, taking the quartz tube out of the heating furnace after the heat preservation is finished, quenching and cooling the quartz tube, placing the quenched and cooled quartz tube into the heating furnace again, heating the quartz tube to 540-560 ℃ from room temperature, preserving the temperature for 3-5 days, and carrying out annealing treatment to obtain the ternary layered selenide Ge 0.85 Bi 2.15+x Se 4 semiconductor material. The invention successfully solves the technical problem that the GeBi 2 Se 4 system is difficult to obtain a single phase by accurately regulating and controlling the Ge/Bi ratio and adopting a high-temperature quenching and low-temperature long-time annealing process.

Inventors

  • MI SHAOBO
  • DING YU
  • ZHANG CHUANLIN
  • LU LU

Assignees

  • 季华实验室

Dates

Publication Date
20260508
Application Date
20260408

Claims (8)

  1. 1. A preparation method of a ternary layered selenide Ge 0.85 Bi 2.15+x Se 4 semiconductor material is characterized by comprising the following steps: S100, taking germanium powder, bismuth powder and selenium powder as raw materials, weighing according to the molar ratio of a chemical formula Ge 0.85 Bi 2.15+x Se 4 , wherein x is more than or equal to 0 and less than or equal to 0.06, uniformly mixing the weighed raw materials, placing the mixture into a quartz tube, vacuumizing the quartz tube, and sealing the quartz tube; S200, placing the quartz tube subjected to vacuum sealing in the step S100 into a heating furnace, heating to 900-950 ℃ from room temperature, preserving heat at the temperature for 12-24 hours, taking out the quartz tube from the heating furnace after the heat preservation is finished, quenching and cooling the quartz tube, and rapidly cooling the quartz tube to the room temperature; S300, placing the quartz tube subjected to quenching and cooling in the step S200 in a heating furnace again, heating to 540-560 ℃ from room temperature, preserving heat for 3-5 days, carrying out annealing treatment, naturally cooling the quartz tube to room temperature along with the furnace after the heat preservation is finished, and then taking out the prepared ternary layered selenide Ge 0.85 Bi 2.15+x Se 4 semiconductor material from the quartz tube.
  2. 2. The method for preparing a ternary layered selenide Ge 0.85 Bi 2.15+x Se 4 semiconductor material according to claim 1, wherein the purity of the germanium powder, bismuth powder and selenium powder is 99.99% or higher.
  3. 3. The method for producing a ternary layered selenide Ge 0.85 Bi 2.15+x Se 4 semiconductor according to claim 1, wherein in step S100, the quartz tube is vacuum-sealed after the pressure in the tube is equal to or less than 1:1 Pa.
  4. 4. The method of claim 1, wherein the quenching in step S200 is performed by rapidly taking the quartz tube out of the furnace and rapidly cooling it in cold water.
  5. 5. The method of manufacturing a ternary layered selenide Ge 0.85 Bi 2.15+x Se 4 semiconductor material according to claim 1, wherein in step S200, the temperature is raised from room temperature to 900-950 ℃ at a rate of 2-5 ℃ per minute.
  6. 6. The method of manufacturing a ternary layered selenide Ge 0.85 Bi 2.15+x Se 4 semiconductor material according to claim 1, wherein in step S300, the temperature is raised from room temperature to 540-560 ℃ at a rate of 2-5 ℃ per minute.
  7. 7. A ternary layered selenide Ge 0.85 Bi 2.15+x Se 4 semiconductor material is characterized in that, a method of preparing a ternary layered selenide Ge 0.85 Bi 2.15+x Se 4 semiconductor material according to any one of claims 1 to 6.
  8. 8. The ternary layered selenide Ge 0.85 Bi 2.15+x Se 4 semiconductor material of claim 7, wherein the ternary layered selenide Ge 0.85 Bi 2.15+x Se 4 semiconductor material has a rhombohedral crystal structure, a space group of R-3m, and exhibits a layered morphology.

Description

Ternary layered selenide Ge 0.85Bi2.15+xSe4 semiconductor material and preparation method thereof Technical Field The invention relates to the technical field of semiconductor material preparation, in particular to a ternary layered selenide Ge 0.85Bi2.15+xSe4 semiconductor material and a preparation method thereof. Background Layered structure chalcogenides are a class of important materials that form three-dimensional periodic crystal structures from two-dimensional or quasi-two-dimensional layered elements stacked in a direction perpendicular to the layer plane. Because the atoms in the layers are combined by strong covalent bonds or metal bonds, and only van der Waals weak interaction exists between the elementary layers, the material has the characteristics of obvious physical and chemical property anisotropism, easy stripping and the like. The unique properties enable the semiconductor device to have wide application prospects in high-performance field effect transistors, photodetectors, gas sensors, spintronics, thermoelectric devices, solar cells and other high and new technical fields. Among the numerous layered chalcogenides, the ternary selenide GeBi 2Se4 is one of the first compounds found in Ge-Bi-Se systems. Research shows that GeBi 2Se4 has rhombohedral crystal structure (space group: R-3 m) and is formed by stacking lamellar structure units along the direction perpendicular to the layer plane. As a narrow bandgap semiconductor material (the band gap is about 0.27 eV), the GeBi 2Se4 has important potential application value in the high-tech fields such as infrared light detection, terahertz wave response, heat energy conversion and the like. However, there are obvious technical drawbacks in the prior art regarding the preparation method of GeBi 2Se4. The preparation technology disclosed at present mainly adopts a method of combining ball milling and vacuum hot-pressing sintering under the protection of argon gas to synthesize the GeBi 2Se4 material. Although this process is capable of obtaining bulk materials, the resultant product often has a hetero-phase rich in germanium (Ge), resulting in a pure phase (single phase) material from which the compound is not obtained. The existence of the impurity phase seriously interferes with the accurate characterization of the intrinsic physical properties of the material and also limits the practical application of the material in high-precision functional devices. Therefore, the method for controllably growing the pure-phase Ge-Bi-Se ternary layered selenide semiconductor is simple and convenient in process, and has important significance for promoting physical property research and application development of the material. Disclosure of Invention In view of the shortcomings of the prior art, the invention aims to provide a ternary layered selenide Ge 0.85Bi2.15+xSe4 semiconductor material and a preparation method thereof, and aims to solve the technical problems that the process is complex and the impurity phase exists in the preparation process of the GeBi 2Se4 material in the prior art. In order to achieve the above purpose, the invention adopts the following technical scheme: a method for preparing a ternary layered selenide Ge 0.85Bi2.15+xSe4 semiconductor material, comprising the steps of: S100, taking germanium powder, bismuth powder and selenium powder as raw materials, weighing according to the molar ratio of a chemical formula Ge 0.85Bi2.15+xSe4, wherein x is more than or equal to 0 and less than or equal to 0.06, uniformly mixing the weighed raw materials, placing the mixture into a quartz tube, vacuumizing the quartz tube, and sealing the quartz tube; S200, placing the quartz tube subjected to vacuum sealing in the step S100 into a heating furnace, heating to 900-950 ℃ from room temperature, preserving heat at the temperature for 12-24 hours, taking out the quartz tube from the heating furnace after the heat preservation is finished, quenching and cooling the quartz tube, and rapidly cooling the quartz tube to the room temperature; S300, placing the quartz tube subjected to quenching and cooling in the step S200 in a heating furnace again, heating to 540-560 ℃ from room temperature, preserving heat for 3-5 days, carrying out annealing treatment, naturally cooling the quartz tube to room temperature along with the furnace after the heat preservation is finished, and then taking out the prepared ternary layered selenide Ge 0.85Bi2.15+xSe4 semiconductor material from the quartz tube. The preparation method of the ternary layered selenide Ge 0.85Bi2.15+xSe4 semiconductor material comprises the step of preparing the ternary layered selenide Ge 0.85Bi2.15+xSe4 semiconductor material, wherein the purities of the germanium powder, the bismuth powder and the selenium powder are all over 99.99 percent. In the preparation method of the ternary layered selenide Ge 0.85Bi2.15+xSe4 semiconductor material, in the step S100, the quartz tube is vacuumized u