CN119637814A - Layered ternary selenide, layered ternary selenide single crystal material and preparation method thereof - Google Patents
Layered ternary selenide, layered ternary selenide single crystal material and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a layered ternary selenide, a layered ternary selenide single crystal material and a preparation method thereof, and belongs to the technical field of crystal materials. The chemical formula of the layered ternary selenide is In 2Ge2Se6, indium powder, germanium powder and selenium powder with specific proportions are adopted as raw materials, and the synthesis of the layered ternary selenide In 2Ge2Se6 single-phase material is realized through high-temperature melting, specific temperature interval heat preservation and quenching processes, the material has a narrow band gap and low heat conductivity, and the thin nano-sheet single-crystal material with millimeter-sized area can be prepared through a mechanical stripping method, so that the layered ternary selenide can be applied to the fields of semiconductor photoelectric devices, solar cells, thermoelectric devices and the like.
Description
Technical Field
The invention relates to the technical field of crystal materials, in particular to a layered ternary selenide, a layered ternary selenide single crystal material and a preparation method thereof.
Background
Chalcogenide compounds of layered structure are numerous and widely used. The compound is formed by stacking two-dimensional or quasi-two-dimensional layered primitives along a certain direction, and van der Waals (VAN DER WAALS) interaction exists between primitive layers, so that the material shows unique physical and chemical properties and has great potential application prospects in the fields of field effect transistors, photoelectric detectors, gas sensors, spintronics, thermoelectric devices and the like.
Wherein, the layered structure A 2M2Q6 (A=in, sb, bi, al, sc, V, cr; M=Si, ge; Q=S, se, te) is taken as a novel material system, and the structure and the performance of the material system are predicted by theoretical calculation. Such materials have unique fermi density, lower lattice thermal conductivity, lower carrier concentration, good kinetic and thermodynamic stability, good ferromagnetic stability, excellent photocatalytic activity, and the like. Notably, part of the predicted material system was experimentally confirmed, such as Sc2Si2Te6,V2Si2Se6,Cr2Ge2Te6 and In 2Ge2Te6. In addition, thin-layer nanoplatelets of such materials exhibit exceptional properties, such as Cr 2Ge2Te6 nanoplatelets exhibiting two-dimensional material properties in the ferromagnetic ground state. For the layered structure In 2Ge2Se6 (space group: R) Theoretical calculation predicts that the semiconductor material has a band gap of about 1.9 eV, and single-layer In 2Ge2Se6 has low heat conductivity, is about 7.68 W.m -1.K-1 at 300K, is expected to be applied to the fields of semiconductor photoelectric devices, solar cells, thermoelectric devices and the like, but no relevant report on experimental synthesis of the material exists at present.
It can be seen that there is a need for improvements and improvements in the art.
Disclosure of Invention
The invention aims to provide a layered ternary selenide, a layered ternary selenide single crystal material and a preparation method thereof, and aims to solve the problem that In 2Ge2Se6 materials with layered structures are synthesized by no technical means In the prior art.
In order to achieve the above purpose, the invention provides the following scheme:
The invention provides a layered ternary selenide, wherein the chemical formula of the layered ternary selenide is In 2Ge2Se6, and the space group of the layered ternary selenide is R 。
A preparation method of a layered ternary selenide single-phase material, wherein the layered ternary selenide is the layered ternary selenide, and the preparation method comprises the following steps:
S001, taking indium powder, germanium powder and selenium powder with the molar ratio of 2:2:6 as raw materials, heating to 950-1000 ℃ under vacuum condition, and preserving heat at the temperature for 12-24 h;
S002, cooling to 650-665 ℃ at a cooling rate of 2-5 ℃ per minute after heat preservation, and preserving heat for 96-240 hours at 650-665 ℃, and quenching and cooling to room temperature after heat preservation, so as to obtain the layered ternary selenide single-phase material with the chemical formula of In 2Ge2Se6.
In the preparation method of the layered ternary selenide single-phase material, in the step S001, the purities of the indium powder, the germanium powder and the selenium powder are all more than or equal to 99.99 percent.
In the preparation method of the layered ternary selenide single-phase material, in the step S001, the vacuum degree of the vacuum condition is less than or equal to 1Pa.
In the preparation method of the layered ternary selenide single-phase material, in the step S001, the temperature rising rate is 2-5 ℃ per minute.
The invention also provides a layered selenium compound single-crystal material, the layered ternary selenium compound single-crystal material is an In 2Ge2Se6 thin-layer nano-sheet, the In 2Ge2Se6 thin-layer nano-sheet is prepared from a layered ternary selenide single-phase material through mechanical stripping, and the layered ternary selenide single-phase material is prepared by the preparation method of the layered ternary selenide single-phase material.
Wherein the In 2Ge2Se6 thin-layer nano-sheet has a layered structure along the direction of the c-axis.
Wherein the lamellar thickness direction of the In 2Ge2Se6 lamellar nano-sheet is the crystallographic c-axis orientation of the In 2Ge2Se6 structure.
The beneficial effects are that:
The invention provides a layered ternary selenide, which has a chemical formula of In 2Ge2Se6, and is prepared by adopting indium powder, germanium powder and selenium powder with specific proportions as raw materials, firing the raw materials at high temperature to enable the indium powder, the germanium powder and the selenium powder to fully react, cooling the raw materials to a certain temperature for heat preservation, and finally quenching the raw materials to obtain the layered ternary selenide single-phase material with the chemical formula of In 2Ge2Se6. The material has a narrower band gap and lower heat conductivity, and can be applied to the fields of semiconductor photoelectric devices, solar cells, thermoelectric devices and the like.
The invention also provides a layered ternary selenide single-crystal material, which is prepared by mechanically stripping the In 2Ge2Se6 single-phase material to obtain a large-area single-crystal thin-layer nano sheet, and provides a material for the research of the intrinsic physical properties of the material and the application In the fields of flexible semiconductor photoelectric devices and the like.
Drawings
Fig. 1 is a photograph taken by an optical microscope of the layered ternary In 2Ge2Se6 selenide single-phase material provided In example 1.
Fig. 2 is an X-ray powder diffraction pattern of the layered ternary In 2Ge2Se6 selenide single phase material provided In example 1.
FIG. 3 is a cross-sectional microscopic morphology scanning electron microscope image of the layered ternary In 2Ge2Se6 selenide single-phase material provided In example 1.
Fig. 4 is an X-ray energy spectrum of the layered ternary In 2Ge2Se6 selenide single phase material provided In example 1.
FIG. 5 is a chart showing the atomic resolution of the layered ternary In 2Ge2Se6 selenide single-phase material provided In example 1 In the [1-100] projection direction.
Fig. 6 is an ultraviolet-visible absorption spectrum of the ternary In 2Ge2Se6 selenide single phase material provided In example 1.
Fig. 7 is thermal conductivity of the ternary In 2Ge2Se6 selenide single phase material provided In example 1 at different temperatures.
Fig. 8 is a photograph of a ternary In 2Ge2Se6 thin-layer nanoplatelet provided In example 1 taken by an optical microscope.
Fig. 9 is an X-ray diffraction pattern of a ternary In 2Ge2Se6 thin-layer nanoplatelet provided In example 1.
Fig. 10 is an X-ray powder diffraction pattern of the layered ternary In 2Ge2Se6 selenide single phase material provided In example 2.
FIG. 11 is an X-ray powder diffraction pattern of the selenide provided in comparative examples 1-3.
Fig. 12 is an X-ray powder diffraction pattern of the selenide provided in comparative example 4, comparative example 5.
Detailed Description
The following description of the embodiments of the present invention will be made clearly and fully with reference to the accompanying drawings, in which it is evident that the embodiments described are only some, but not all embodiments of the invention. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
In a first aspect, the present invention provides a layered ternary selenide having the formula In 2Ge2Se6, a space group RTests show that the band gap of the layered ternary selenide is 1.43 eV, the thermal conductivity at 300K is 2.42 W.m -1.K-1, and the layered ternary selenide has a narrower band gap and a lower thermal conductivity, so that the layered ternary selenide can be applied to the fields of semiconductor photoelectric devices, solar cells, thermoelectric devices and the like, and has a good application prospect.
The second aspect of the invention provides a preparation method of a layered ternary selenide single-phase material, which comprises the following steps:
S001, taking indium powder, germanium powder and selenium powder with the molar ratio of 2:2:6 as raw materials, uniformly mixing the indium powder, the germanium powder and the selenium powder, then placing the mixture into a quartz tube, sealing the quartz tube filled with the raw materials by using flame sealing equipment under a vacuum condition, vertically placing the sealed quartz tube into a single-temperature zone pit furnace, heating the sealed quartz tube to 950-1000 ℃, and preserving the temperature for 12-24 hours at the temperature to fully react the raw materials in the quartz tube;
S002, cooling from 950-1000 ℃ to 650-665 ℃ at a cooling rate of 2-5 ℃ per minute after heat preservation is finished, and preserving heat for 96-240 hours at 650-665 ℃, and quenching and cooling to room temperature after heat preservation is finished, so as to obtain the layered ternary In 2Ge2Se6 single-phase material.
According to the preparation method of the layered ternary selenide single-phase material, indium powder, germanium powder and selenium powder which are prepared In a specific ratio are used as raw materials, the indium powder, the germanium powder and the selenium powder are fully reacted through high-temperature firing, and through quenching treatment, particularly heat preservation treatment is carried out at 650-665 ℃ and a proper cooling rate is selected, the formation of In 2Ge2Se6 seed crystals and nucleation growth can be promoted, and the layered ternary selenide single-phase material with a larger size is obtained.
In the above preparation method, since the purities of the indium powder, the germanium powder and the selenium powder affect the formation of the layered ternary selenide single-phase material, in a preferred embodiment, in the step S001, the purities of the indium powder, the germanium powder and the selenium powder are all equal to or greater than 99.99%, and by adopting the high-purity raw materials, the influence of impurities In the raw materials on the growth of In 2Ge2Se6 seed crystals can be reduced, so that the product does not contain other non-In 2Ge2Se6 crystal phases.
In addition, in the preparation method, the vacuum degree can also influence the formation of the single-phase material in the firing process, and the higher the vacuum degree is, the smaller the influence of air on crystals is, and the lower the possibility of impurity phase occurrence of the formed single-phase body is. In a preferred embodiment, in this regard, in the step S001, the influence of air on the high-temperature firing is reduced by controlling the vacuum degree to be 1Pa or less, so that a layered In 2Ge2Se6 single-phase material is obtained.
In addition, in the aforementioned production method, the rate of temperature rise in step S001 also affects the purity of the material, and when the rate of temperature rise is too high, a phenomenon of component segregation is likely to occur. In a preferred embodiment, in the step S001, the heating rate is controlled to be 2-5 ℃ per min, so that each raw material is heated uniformly, the phenomenon of component segregation is avoided, and the lamellar In 2Ge2Se6 single-phase material is obtained.
The third aspect of the invention also provides a layered ternary selenide single-phase material, which is an In 2Ge2Se6 thin-layer nano-sheet, has a layered structure along the c-axis direction, the crystallographic c-axis direction is the lamellar thickness direction of the In 2Ge2Se6 thin-layer nano-sheet, the layered ternary selenide single-phase material prepared by the method can be prepared by a mechanical stripping mode, for example, an In 2Ge2Se6 thin-layer nano-sheet or a few-layer two-dimensional material can be stripped from the layered In 2Ge2Se6 single-phase material by a tape pasting or repeated pasting mode, and the In 2Ge2Se6 thin-layer nano-sheet or the few-layer two-dimensional material is a single-crystal material, so that materials are provided for subsequent researches on the intrinsic physical properties of the In 2Ge2Se6 selenide and the fields of semiconductor flexible photoelectric devices, solar cells, thermoelectric devices and the like.
To further illustrate the layered ternary selenide provided by the present invention, and methods of preparing a single phase material and a single crystal material thereof, the following examples and comparative examples are provided.
Example 1
The embodiment provides a preparation method of a layered ternary selenide single-phase material, which comprises the following steps:
S001, adopting indium powder with the purity of 99.99%, germanium powder with the purity of 99.99% and selenium powder with the purity of 99.99% and the mol ratio of 2:2:6 as raw materials, uniformly mixing the indium powder, the germanium powder and the selenium powder in a quartz tube, sealing the quartz tube filled with the raw materials by using flame sealing equipment under the condition that the vacuum degree is less than or equal to 1Pa, vertically placing the vacuum-sealed quartz tube in a single-temperature-zone pit furnace, heating the quartz tube close to a thermocouple from room temperature to 950 ℃ at 5 ℃ per minute, and preserving heat for 12 hours at the temperature to fully react the raw materials in the quartz tube;
s002, after heat preservation, quenching the material In the quartz tube, specifically, cooling from 950 ℃ to 665 ℃ at a cooling rate of 2 ℃ per minute, and preserving heat at the temperature for 96 hours;
S003, mechanically stripping the layered ternary In 2Ge2Se6 single-phase material, and repeatedly pasting the layered ternary In 2Ge2Se6 single-phase material through an adhesive tape to obtain the In 2Ge2Se6 thin-layer single-crystal nano-sheet.
The morphology, chemical composition and structure of the lamellar ternary In 2Ge2Se6 single-phase material prepared In example 1 are analyzed and characterized by an optical microscope, an X-ray diffractometer, a scanning electron microscope, an X-ray energy spectrometer and a transmission electron microscope, and specific characterization results are shown In figures 1 to 5. Wherein, according to a 2M2Q6 structural model (Journal of Semiconductors, 44 (2023) 042101) given by theoretical prediction, the layered ternary In 2Ge2Se6 single-phase material obtained In example 1 is determined to be a single-phase material by analyzing an X-ray energy spectrum (fig. 4) and an X-ray powder diffraction spectrum (fig. 2), and the chemical composition of the single-phase material is In 2Ge2Se6.
As can be seen from the scanning electron microscope morphology graph of FIG. 3, the lamellar ternary In 2Ge2Se6 single-phase material macrostructure obtained In example 1 has lamellar morphology features. The high angle annular dark field image obtained by using a transmission electron microscope further shows that the crystal structure of the obtained lamellar ternary In 2Ge2Se6 material is consistent with that of an A 2M2Q6 structural model (Journal of Semiconductors, 44 (2023) 042101), and has a lamellar structure along the c-axis direction.
The layered ternary selenide single-phase material prepared in example 1 was tested for its optical bandgap (fig. 6) and thermal conductivity (fig. 7) by testing its uv-vis absorption spectrum and thermal diffusivity. The optical band gap of the material is 1.43 eV, and the thermal conductivity of the material at 300K is 2.42 W.m -1.K-1.
In addition, the morphology and structure of the In 2Ge2Se6 thin-layer nanoplatelets obtained In example 1 were characterized by a light microscope and an X-ray diffractometer, and the characterization results are shown In FIG. 8 and FIG. 9, and it can be seen from FIG. 8 that the In 2Ge2Se6 thin-layer nanoplatelets can be obtained by a mechanical peeling method using repeated sticking of adhesive tapes, while by indexing the X-ray powder diffraction pattern (FIG. 9) thereof, the (000 l) (l=3, 6, 9) crystal face of the structure of In 2Ge2Se6 corresponding to the diffraction peak was determined, indicating that the obtained In 2Ge2Se6 thin-layer nanoplatelets were single crystal materials and the crystallographic c-axis orientation of the structure of In 2Ge2Se6 In the thickness direction of the lamellae.
Example 2
The embodiment provides a preparation method of a layered ternary selenide single-phase material, which comprises the following steps:
S001, adopting indium powder with the purity of 99.99%, germanium powder with the purity of 99.99% and selenium powder with the purity of 99.99% and the mol ratio of 99.99% to 2:6 as raw materials, uniformly mixing the indium powder, the germanium powder and the selenium powder into a quartz tube, sealing the quartz tube filled with the raw materials by using flame sealing equipment under the condition that the vacuum degree is less than or equal to 1Pa, vertically placing the vacuum sealed quartz tube in a single-temperature-zone pit furnace, heating the quartz tube close to a thermocouple from room temperature to 1000 ℃ at 5 ℃ per min, and preserving heat for 12 hours at the temperature to melt the raw materials in the quartz tube;
S002, after heat preservation, quenching the material In the quartz tube, specifically, cooling from 1000 ℃ to 650 ℃ at a cooling rate of 5 ℃ per minute, preserving heat at the temperature for 240 hours, and then quenching and cooling to room temperature to obtain the layered ternary In 2Ge2Se6 single-phase material.
The morphology, chemical composition and structure of the obtained material are analyzed and characterized by an optical microscope, an X-ray diffractometer, a scanning electron microscope and an X-ray energy spectrometer, wherein the X-ray powder diffraction pattern is shown In figure 10, and as can be seen from figure 8, the characteristic diffraction peaks of other phases do not appear In the X-ray powder diffraction pattern, which indicates that the lamellar ternary In 2Ge2Se6 single-phase material prepared In example 2 is a single-phase material. In addition, since the surface topography and structure are the same as those of example 1, the relevant drawings are not shown.
Comparative example 1
The comparative example provides a method for preparing selenide comprising the following steps:
S001, adopting indium powder with the purity of 99.99%, germanium powder with the purity of 99.99% and selenium powder with the purity of 99.99% and the mol ratio of 99.99% to 2:6 as raw materials, uniformly mixing the indium powder, the germanium powder and the selenium powder in a quartz tube, sealing the quartz tube filled with the raw materials by using flame sealing equipment under the condition that the vacuum degree is less than or equal to 1Pa, vertically placing the vacuum-sealed quartz tube in a single-temperature-zone pit furnace, heating the quartz tube close to a thermocouple from room temperature to 950 ℃ at 5 ℃ per min, and preserving heat for 12 hours at the temperature to fully react the raw materials in the quartz tube;
And S002, after the heat preservation is finished, directly quenching the material in the quartz tube (water-cooling to room temperature), and then taking out the material from the quartz tube.
The phase structure of the material obtained In comparative example 1 was analyzed and characterized by an X-ray diffractometer, the characterization result is shown In fig. 9, and as seen from fig. 11, the X-ray powder diffraction pattern of the material obtained In comparative example 1 shows characteristic diffraction peaks of other phases, the material obtained In comparative example 1 includes In 2Ge2Se6 phase and a small amount of In 2Se3 phase (characteristic diffraction peak is shown by arrow) and GeSe 2 phase (characteristic diffraction peak is shown by solid circle), and no In 2Ge2Se6 single-phase material was obtained.
Comparative example 2
The comparative example provides a method for preparing selenide comprising the following steps:
S001, adopting indium powder with the purity of 99.99%, germanium powder with the purity of 99.99% and selenium powder with the purity of 99.99% and the mol ratio of 99.99% to 2:6 as raw materials, uniformly mixing the indium powder, the germanium powder and the selenium powder in a quartz tube, sealing the quartz tube filled with the raw materials by using flame sealing equipment under the condition that the vacuum degree is less than or equal to 1Pa, vertically placing the vacuum-sealed quartz tube in a single-temperature-zone pit furnace, heating the quartz tube close to a thermocouple from room temperature to 950 ℃ at 5 ℃ per min, and preserving heat for 12 hours at the temperature to fully react the raw materials in the quartz tube;
s002, after heat preservation, quenching the material in the quartz tube, specifically, cooling from 950 ℃ to 680 ℃ at a cooling rate of 2 ℃ per minute, and preserving heat at the temperature for 96 hours, then quenching and cooling to room temperature, and then taking out the material from the quartz tube.
The phase structure of the material obtained In comparative example 2 was analyzed and characterized by an X-ray diffractometer, the characterization result is shown In fig. 11, and as seen from fig. 9, the X-ray powder diffraction pattern of the material obtained In comparative example 2 shows characteristic diffraction peaks of other phases, the material obtained In comparative example 2 includes In 2Ge2Se6 phase and In 2Se3 phase (characteristic diffraction peaks are shown by arrows), and no In 2Ge2Se6 single-phase material was obtained.
Comparative example 3
The comparative example provides a method for preparing selenide comprising the following steps:
S001, adopting indium powder with the purity of 99.99%, germanium powder with the purity of 99.99% and selenium powder with the purity of 99.99% and the mol ratio of 99.99% to 2:6 as raw materials, uniformly mixing the indium powder, the germanium powder and the selenium powder in a quartz tube, sealing the quartz tube filled with the raw materials by using flame sealing equipment under the condition that the vacuum degree is less than or equal to 1Pa, vertically placing the vacuum-sealed quartz tube in a single-temperature-zone pit furnace, heating the quartz tube close to a thermocouple from room temperature to 950 ℃ at 5 ℃ per min, and preserving heat for 24 hours at the temperature to fully react the raw materials in the quartz tube;
s002, after heat preservation, quenching the material in the quartz tube, specifically, cooling from 950 ℃ to 640 ℃ at a cooling rate of 2 ℃ per minute, and preserving heat at the temperature for 240 hours, then quenching and cooling to room temperature, and then taking out the material from the quartz tube.
The phase structure of the material obtained In comparative example 3 was analyzed and characterized by an X-ray diffractometer, the characterization result is shown In fig. 9, and as seen from fig. 11, the X-ray powder diffraction pattern of the material obtained In comparative example 3 shows characteristic diffraction peaks of other phases, the material obtained In comparative example 3 includes In 2Ge2Se6 phase and a small amount of In 2Se3 phase (characteristic diffraction peaks are shown by arrows), and no In 2Ge2Se6 single-phase material was obtained.
As is clear from comparative examples 1,2 and 3, in 2Ge2Se6 single-phase material can be obtained only by a specific holding temperature range and holding time when quenching treatment is performed.
Comparative example 4
The comparative example provides a method for preparing selenide comprising the following steps:
S001, adopting indium powder with the purity of 99.99%, germanium powder with the purity of 99.99% and selenium powder with the purity of 99.99% and the molar ratio of 99.99% to 2.05 to 6 as raw materials, uniformly mixing the indium powder, the germanium powder and the selenium powder in a quartz tube, sealing the quartz tube filled with the raw materials by using flame sealing equipment under the condition that the vacuum degree is less than or equal to 1Pa, vertically placing the vacuum-sealed quartz tube in a single-temperature zone pit furnace, heating the quartz tube close to a thermocouple from room temperature to 950 ℃ at 5 ℃ per min, and preserving heat for 24 hours at the temperature to fully react the raw materials in the quartz tube;
S002, after heat preservation, quenching the material in the quartz tube, specifically, cooling from 950 ℃ to 665 ℃ at a cooling rate of 2 ℃ per minute, and preserving heat at the temperature for 96 hours, then quenching and cooling to room temperature, and then taking out the material from the quartz tube.
The phase structure of the material obtained In comparative example 4 was analyzed and characterized by an X-ray diffractometer, the characterization result is shown In fig. 10, and as seen from fig. 12, the X-ray powder diffraction pattern of the material obtained In comparative example 4 shows characteristic diffraction peaks of other phases, the material obtained In comparative example 4 includes not only In 2Ge2Se6 phase but also In 2Se3 phase (characteristic diffraction peak is shown by arrow) and other unknown phases (characteristic diffraction peak is shown by triangle symbol), and no In 2Ge2Se6 single-phase material was obtained.
Comparative example 5
The comparative example provides a method for preparing selenide comprising the following steps:
S001, adopting indium powder, germanium powder and selenium powder with the purity of 99.99 percent, 99.99 percent and 99.99 percent, taking the indium powder, the germanium powder and the selenium powder with the molar ratio of 2:1.95:6 as raw materials, uniformly mixing the indium powder, the germanium powder and the selenium powder into a quartz tube, sealing the quartz tube filled with the raw materials by using flame sealing equipment under the condition that the vacuum degree is less than or equal to 1Pa, vertically placing the quartz tube which is already sealed in a single-temperature zone pit furnace, heating the quartz tube to 950 ℃ from room temperature at 5 ℃ per min near a thermocouple, and preserving heat for 24 hours at the temperature to enable the raw materials in the quartz tube to fully react;
s002, after heat preservation, quenching the material in the quartz tube, specifically, cooling from 950 ℃ to 665 ℃ at a cooling rate of 2.5 ℃ per minute, and preserving the heat at the temperature for 96 hours, then quenching and cooling to room temperature, and then taking out the material from the quartz tube.
The phase structure of the material obtained In comparative example 5 was analyzed and characterized by an X-ray diffractometer, the characterization result is shown In fig. 12, and as seen from fig. 12, the X-ray powder diffraction pattern of the material obtained In comparative example 5 shows characteristic diffraction peaks of other phases, the material obtained In comparative example 5 includes In 2Ge2Se6 phase and a small amount of In 2Se3 phase (characteristic diffraction peaks are shown by arrows), and no In 2Ge2Se6 single-phase material was obtained.
From comparative examples 4 and 5, it is known that the layered ternary In 2Ge2Se6 single-phase material can be obtained by precisely controlling the dosage ratio of indium powder, germanium powder and selenium powder.
In conclusion, the preparation method of the layered ternary selenide single-phase material can be used for preparing the layered ternary selenide single-phase material with the chemical formula of In 2Ge2Se6, expands a material system which can be synthesized by the layered structure A 2M2Q6, and provides material support for further physical property research and device development and application of the layered structure A 2M2Q6 material system. In the lamellar ternary In 2Ge2Se6 single-phase material prepared by the method, an In 2Ge2Se6 lamellar nano sheet with millimeter-scale area or a few-layer two-dimensional single-crystal material can be obtained by a mechanical stripping mode, and the material is provided for the research of intrinsic physical properties of the material under the condition of few-layer two-dimensional and the application In the fields of flexible semiconductor photoelectric devices, solar cells, thermoelectric devices and the like.
The foregoing description is only of the preferred embodiments of the present invention and is not intended to limit the scope of the invention, and all equivalent structural changes made by the description of the present invention and the accompanying drawings or direct/indirect application in other related technical fields are included in the scope of the invention.
Claims (8)
1. A layered ternary selenide is characterized In that the chemical formula is In 2Ge2Se6, and the space group is R。
2. A method for preparing a layered ternary selenide single-phase material, wherein the layered ternary selenide is the layered ternary selenide according to claim 1, and the method comprises the following steps:
S001, taking indium powder, germanium powder and selenium powder with the molar ratio of 2:2:6 as raw materials, heating to 950-1000 ℃ under vacuum condition, and preserving heat at the temperature for 12-24 h;
S002, cooling to 650-665 ℃ at a cooling rate of 2-5 ℃ per minute after heat preservation, and preserving heat for 96-240 hours at 650-665 ℃, and quenching and cooling to room temperature after heat preservation, so as to obtain the layered ternary selenide single-phase material with the chemical formula of In 2Ge2Se6.
3. The method for preparing the layered ternary selenide single-phase material according to claim 2, wherein in the step S001, the purities of the indium powder, the germanium powder and the selenium powder are all equal to or higher than 99.99%.
4. The method for preparing a layered ternary selenide single-phase material according to claim 2, wherein in step S001, the vacuum degree of the vacuum condition is equal to or less than 1Pa.
5. The method for preparing a layered ternary selenide single-phase material according to claim 2, wherein in step S001, the temperature rising rate is 2-5 ℃.
6. A layered ternary selenide single-crystal material, characterized In that the layered ternary selenide single-crystal material is an In 2Ge2Se6 thin-layer nano-sheet, the In 2Ge2Se6 thin-layer nano-sheet is prepared from a layered ternary selenide single-phase material by mechanical stripping, and the layered ternary selenide single-phase material is prepared by the preparation method of the layered ternary selenide single-phase material according to any one of claims 2 to 5.
7. The layered ternary selenium compound single crystal material of claim 6, wherein the In 2Ge2Se6 thin layer nanoplatelets have a layered structure along the c-axis direction.
8. The layered ternary selenium compound single crystal material of claim 7, wherein the lamellar thickness direction of the In 2Ge2Se6 lamellar nanoplatelets is the crystallographic c-axis orientation of the In 2Ge2Se6 structure.
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|---|---|---|---|---|
| CN120736476A (en) * | 2025-09-08 | 2025-10-03 | 季华实验室 | Ternary layered selenide Ge3Sb4Se7Semiconductor material and preparation method thereof |
| CN120945476A (en) * | 2025-10-16 | 2025-11-14 | 季华实验室 | A large-size ternary layered In2Ge2Se6 single crystal material and its preparation method |
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| US6169245B1 (en) * | 1998-05-05 | 2001-01-02 | Marlow Industries, Inc. | Thermoelectric materials ternary penta telluride and selenide compounds |
| CN117822122A (en) * | 2024-03-05 | 2024-04-05 | 季华实验室 | A layered Ge1-xSb4+xTe7 single crystal and preparation method thereof |
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| US6169245B1 (en) * | 1998-05-05 | 2001-01-02 | Marlow Industries, Inc. | Thermoelectric materials ternary penta telluride and selenide compounds |
| CN117822122A (en) * | 2024-03-05 | 2024-04-05 | 季华实验室 | A layered Ge1-xSb4+xTe7 single crystal and preparation method thereof |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN120736476A (en) * | 2025-09-08 | 2025-10-03 | 季华实验室 | Ternary layered selenide Ge3Sb4Se7Semiconductor material and preparation method thereof |
| CN120945476A (en) * | 2025-10-16 | 2025-11-14 | 季华实验室 | A large-size ternary layered In2Ge2Se6 single crystal material and its preparation method |
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