CN114855282A - Silicon ditelluride two-dimensional crystal material and preparation method thereof - Google Patents
Silicon ditelluride two-dimensional crystal material and preparation method thereof Download PDFInfo
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- 229910052710 silicon Inorganic materials 0.000 title claims abstract description 44
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 title claims abstract description 43
- 239000010703 silicon Substances 0.000 title claims abstract description 41
- JPIIVHIVGGOMMV-UHFFFAOYSA-N ditellurium Chemical compound [Te]=[Te] JPIIVHIVGGOMMV-UHFFFAOYSA-N 0.000 title claims abstract description 15
- 238000002360 preparation method Methods 0.000 title claims abstract description 13
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- PORWMNRCUJJQNO-UHFFFAOYSA-N tellurium atom Chemical group [Te] PORWMNRCUJJQNO-UHFFFAOYSA-N 0.000 claims description 23
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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
-
- 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
- C30B25/00—Single-crystal growth by chemical reaction of reactive gases, e.g. chemical vapour-deposition growth
- C30B25/02—Epitaxial-layer growth
- C30B25/18—Epitaxial-layer growth characterised by the substrate
- C30B25/186—Epitaxial-layer growth characterised by the substrate being specially pre-treated by, e.g. chemical or physical means
-
- 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
- C30B29/60—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape characterised by shape
- C30B29/64—Flat crystals, e.g. plates, strips or discs
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P70/00—Climate change mitigation technologies in the production process for final industrial or consumer products
- Y02P70/50—Manufacturing or production processes characterised by the final manufactured product
Abstract
Provides a two-dimensional crystal thin film material of silicon ditelluride and a preparation method thereof. According to one embodiment, the preparation method comprises the following steps: 1) under the vacuum condition, rapidly heating and rapidly cooling the silicon single crystal to obtain a reformed surface; 2) high purity Te was deposited onto the substrate surface by an evaporation source. During the deposition process, the silicon single crystal substrate is kept at a set temperature, so that Te and Si single crystals fully react to form a two-dimensional crystal film SiTe with a periodic structure 2 . The lattice arrangement period of the novel two-dimensional material can be determined by low-energy electron diffraction. The invention directly grows the two-dimensional crystal film SiTe by taking the silicon substrate as a reaction material 2 The method expands the research field of two-dimensional atomic crystal materials and has wide application potential in the field of future nano electronics.
Description
Technical Field
The application belongs to the technical field of nano materials, and particularly relates to a novel two-dimensional crystal thin film material silicon ditelluride (SiTe) 2 ) And a method for preparing the material.
Background
Since the discovery of graphene in 2004, two-dimensional materials have since been uncovered with veil. Graphene, as a representative of two-dimensional materials, exhibits excellent properties such as mechanical characteristics with high strength, having 15000cm at room temperature 2 The carrier mobility of/V.s, and excellent heat conduction performance. This makes graphene an attractive material, which has been a global research hotspot in recent years.
In the application of semiconductor chips, graphene lacks of natural semiconductor band gaps, so that the application of graphene in the fields of semiconductors and the like is limited. Researchers have developed the exploration and study of other new two-dimensional materials. In recent years, experimental and theoretical researches find that other graphene-like two-dimensional atomic crystal materials, such as molybdenum disulfide, silylene, stannene, boron nitride and the like, continuously expand databases of two-dimensional materials. These two-dimensional materials also exhibit a variety of novel physical properties of electrical, thermal, magnetic, etc.
The Si-Te system is also a novel two-dimensional material explored by researchers, and SiTe is predicted according to theory 2 Possibility exists and it is predicted that it has excellent properties: has extremely low lattice heat conductivity coefficient and good electronic property. Therefore, the electrode has potential application prospect in the fields of thermoelectricity, flexible electrodes and the like. At present, no experiment report about two-dimensional SiTe is reported in the aspect of material preparation 2 And (4) synthesizing materials. As a brand new two-dimensional crystal material, the successful preparation of the crystal material is a precondition for further development of physical property research and application development. Thus, the two-dimensional crystal material SiTe is prepared by a feasible method 2 It is very important.
Disclosure of Invention
In view of this,the invention aims to provide a method for preparing two-dimensional crystal SiTe 2 A method of forming a thin film material. By the method of the present invention, a novel two-dimensional material can be prepared, which exhibits a two-dimensional periodic structure of a triangular lattice arrangement.
One aspect of the present invention provides a method for preparing SiTe 2 A method of forming a film material, comprising the steps of:
processing a single crystal substrate in a vacuum environment to obtain a reconstructed surface, wherein the single crystal substrate is a silicon single crystal; and
and evaporating and depositing tellurium atoms onto the single crystal substrate, and keeping the single crystal substrate at a set temperature so that tellurium and silicon react with each other to form a two-dimensional crystal material with a periodic structure.
In some examples, processing the single crystal substrate includes:
heating the single crystal substrate in vacuum at a heating rate of more than 400 ℃/s;
preserving the heat of the heated single crystal substrate for a preset time; and
the single crystal substrate is cooled to obtain a reconstituted surface.
In some examples, the reconstituted silicon single crystal surface is a Si (111)7 × 7 structure.
In some examples, the set temperature is 350-.
In some examples, the evaporation deposition is resistive heating evaporation deposition and/or electron beam evaporation deposition.
In some examples, the resistive heating evaporation deposition is performed as follows: the resistance wire is electrified and heated to heat the evaporation source to a preset temperature so as to evaporate tellurium atoms, and the evaporated tellurium atoms form beam current to be deposited on the substrate.
In some examples, the deposition time is 5-20 minutes.
In some examples, the method of making further comprises: and slowly cooling the two-dimensional crystal material obtained after deposition to room temperature.
The invention provides a silicon ditelluride two-dimensional crystal material, which is characterized in that crystal atoms are arranged in a triangular periodic manner and are orderly expanded in a two-dimensional plane to form a silicon ditelluride film material.
In some examples, the lattice period of the silicon ditelluride thin film material is 0.44nm, which is characterized by low energy electron diffraction.
The invention prepares the two-dimensional atomic crystal thin film material SiTe by a molecular beam epitaxy method 2 The grown thin films are periodically arranged in a triangular shape on the whole surface of the silicon single crystal, and the arrangement can be known from a low-energy electron diffraction pattern. Prepared SiTe 2 As a new two-dimensional material, the compound of the existing two-dimensional material is expanded, and a foundation is laid for further carrying out physical property research and application development on the compound of the two-dimensional material, for example, the compound of the two-dimensional material theoretically has extremely low lattice thermal conductivity and good electronic performance, so that the compound of the two-dimensional material has application potential in field effect transistors, flexible photoelectric devices and the like.
Drawings
In order to more clearly illustrate the embodiment of the present invention or the technical solutions in the prior art, the drawings used in the embodiment will be briefly described below.
FIG. 1 shows a two-dimensional crystal SiTe according to an exemplary embodiment of the present application 2 The preparation process of the film material is shown schematically.
FIG. 2 illustrates the preparation of a two-dimensional crystal SiTe according to an exemplary embodiment of the present application 2 A flow chart of a method of thin film materials.
FIG. 3 illustrates the preparation of SiTe for growth used in an exemplary embodiment of the present application 2 High quality single crystal Si (111) surface and two-dimensional crystal SiTe of thin film 2 Low energy electron diffraction pattern of the film.
FIG. 4 illustrates a simulated SiTe in an exemplary embodiment of the present application 2 Low energy electron diffraction pattern of the thin film.
FIG. 5 shows a single layer of SiTe 2 The atomic structure model of (1).
Detailed Description
Hereinafter, exemplary embodiments of the present application will be described in detail with reference to the accompanying drawings. It should be understood that the described embodiments are only some embodiments of the present application and not all embodiments of the present application, and that the present application is not limited by the example embodiments described herein. Unless defined otherwise, technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art.
As previously mentioned, although two-dimensional SiTe is predicted by calculation 2 The prior art only prepares bulk materials, and does not disclose a successful preparation method for realizing two-dimensional materials. For this purpose, the invention obtains SiTe through molecular beam epitaxial growth 2 Fig. 1 shows a schematic view of a manufacturing process of an exemplary embodiment of the present application. As shown in FIG. 1, two-dimensional SiTe having an ordered structure can be formed on the surface of a silicon single-crystal substrate by introducing Te atoms of an evaporation source to the surface of the silicon single-crystal substrate and maintaining the temperature of the surface of the substrate at a predetermined temperature 2 A crystalline thin film material.
FIG. 2 illustrates the preparation of two-dimensional crystal SiTe according to an embodiment of the present application 2 A flow chart of a method of thin film materials.
Referring to fig. 2, the production method 10 may begin with step S12 in which a silicon single crystal substrate is processed to obtain a reconstituted surface.
In order to avoid the introduction of impurities, the steps of the production process of the present invention are preferably carried out under vacuum. For example, a silicon single crystal may be surface-treated in an ultra-high vacuum environment to obtain a clean and flat surface. Specifically, the vacuum environment refers to a vacuum degree of 10 -10 -10 -7 mbar, e.g. by molecular pump, to a vacuum of 2-6X 10 -10 mbar, the gas molecules adsorbed in the silicon substrate can be effectively removed by adopting the vacuum environment, so that adverse effects of the gas molecules on subsequent Te and Si reactions are avoided.
In the present invention, the single crystal silicon is used as a substrate and a raw material participating in the reaction, and the single crystal silicon having a purity of 99.99% or more can be selected as a substrate material. When the silicon single crystal is not processed well, the surface has a disordered structure, and no diffraction spots can be seen in low-energy electron diffraction. In order to produce a two-dimensional material, the surface of single crystal silicon needs to be treated to obtain an atomically flat surface.
In one embodiment, the silicon substrate may be processed by rapid heating and then rapid cooling, for example, heating the single crystal silicon substrate in a vacuum deposition chamber at a heating rate of more than 400 ℃/s, preferably more than 600 ℃/s, for example, by heating the silicon substrate to 1100 ℃/s within 2 seconds, then maintaining the heated single crystal substrate at the temperature for a predetermined time, for example, for 5 to 10 seconds, and then cooling the single crystal substrate to obtain a reconstructed surface, for example, by reducing the current flowing through the silicon single crystal and reducing the current to zero within a short time, and rapidly cooling the single crystal substrate. By this way of processing, a reconstructed ordered surface structure can be obtained.
In one embodiment, a Si (111) single crystal is used as a substrate material, which is heated by energization in vacuum, the substrate temperature is raised to 1200 ℃ within 2 seconds, then maintained for 6 seconds, and then the current applied to the Si single crystal is reduced to zero for 2 seconds, so that it is naturally cooled. As shown in fig. 3a, by analyzing the low-energy electron diffraction pattern, it was confirmed that the substrate surface obtained in this manner had a 7 × 7 Si (111) crystal structure, which was advantageous for the subsequent molecular beam epitaxial growth.
After the silicon substrate is processed, the process may continue with step S14 in which tellurium atoms are vapor deposited onto the single crystal substrate and the single crystal substrate is maintained at a set temperature such that the tellurium and silicon react with each other to form a two-dimensional crystal material having a periodic structure.
Experiments show that tellurium and silicon can not react to form SiTe at any temperature 2 Or the reaction product is a crystal film of an atomic layer, so the reaction temperature of the two needs to be controlled, and the inventor finds that the ideal two-dimensional film material can be prepared only by controlling the reaction temperature at 350-. If the temperature is less than 350 c, tellurium may form a passivation layer on the surface to make it difficult to sufficiently react Te with Si single crystal to be distributed over the entire silicon single crystal substrate, while if the temperature exceeds 400 c, it is difficult to obtain a two-dimensional crystal structure of a desired composition. Preferably, the reaction temperature is controlled at 360-375 ℃, which can form a two-dimensional material with better quality.
To control the reaction temperature, the substrate surface may be heated by direct current and maintained at the reaction temperature during deposition. The heating step may be performed prior to the step of heating and evaporating the tellurium source to prevent tellurium from being deposited on the surface of the silicon substrate below the above reaction temperature. To avoid the influence of impurities, a tellurium source with high purity can be selected, for example, the purity of the tellurium source is more than 95%.
In one embodiment, Te atoms can be deposited on the surface of Si (111) by resistance heating evaporation deposition, for example, tellurium atoms can be evaporated by heating an evaporation source to a predetermined temperature by heating a resistance wire, and the evaporated tellurium atoms are deposited on a substrate to form a beam to form a two-dimensional SiTe with an ordered structure 2 And (5) a crystal thin film. The temperature of the evaporation source can be controlled to be lower than the heating temperature of the monocrystalline silicon substrate, so that the reaction process of Si and Te can be controlled and better SiTe can be obtained 2 Crystallinity, preferably, the resistance heating (K-cell) evaporation source can be heated to 220-250 ℃. When an evaporation source with a purity not too high (for example, the purity of the tellurium source is below 95%) is used, the temperature of the evaporation source is especially controlled to avoid evaporating impurities to affect the quality of the two-dimensional thin film material, and more preferably, the temperature is controlled to 230 ℃ and 235 ℃. The entire deposition process lasts for about 5-20 minutes, for example 10 minutes.
In another embodiment, an electron beam evaporation source may be used as the Te source. For example, high voltage is applied to the emitted electrons generated by the electrified wire to generate electron beams to accelerate and bombard the tellurium source and sublimate the tellurium source, the tellurium atom evaporation source formed by sublimation forms a beam under the constraint of an evaporation source opening and deposits the beam on the silicon substrate, and two-dimensional SiTe can also be obtained 2 And (5) a crystal thin film.
After completing the deposition of the tellurium atoms to obtain the two-dimensional thin film material, the fabrication method may further proceed to step S16 to cool the two-dimensional crystal material on the substrate.
In one embodiment, the temperature of the silicon single crystal substrate can be slowly lowered, for example, cooled to room temperature by natural cooling, and the whole temperature lowering process is about 20 minutes. After cooling to room temperature, the two-dimensional material is shown to have an ordered structure on a macroscopic scale by a low-energy electron diffraction pattern, namely the prepared two-dimensional material is distributed on the whole silicon single crystalOn a substrate. As shown in FIG. 3b, in which the 7X 7 structure of the Si (111) surface disappears, leaving only the 1X 1 structure of the Si (111) surface, the other diffraction points (2V 3X 2V 3) are derived from the surface two-dimensional material SiTe as shown by the circled portion in the figure 2 The contribution of (c).
In the exemplary embodiment, the atomic-level silicon ditelluride two-dimensional material film layer is obtained by the preparation method, the current situation that only a blocky body can be obtained in the prior art is solved, and a foundation can be provided for developing physical property research of silicon ditelluride and application and development of related devices.
Another embodiment of the present invention provides a two-dimensional crystalline silicon ditelluride material, which can be prepared, for example, by the method described above, as shown in FIG. 3b, and the obtained SiTe is prepared 2 The crystal atoms are arranged in a triangular periodic manner and are orderly expanded in a two-dimensional plane, so that the silicon ditelluride film material can be formed.
For clarity of the description of the low energy electron diffraction pattern of FIG. 3b, FIG. 4 shows a simulated SiTe 2 Low energy electron diffraction pattern of the thin film. As shown in fig. 4a, which depicts a schematic diagram of diffraction points of a two-dimensional material fabricated on a silicon single crystal substrate. The Si (111) diffraction points are indicated by white dots, and the new diffraction points are indicated by gray dots. According to the relationship of the reciprocal lattice vectors, the lattice arrangement in the real space can be reversely deduced, and the formed SiTe can be determined in the real space 2 The lattice period of the film is shown in fig. 4 b. Here, gray arrows indicate lattice vectors of Si (111), and black arrows indicate lattice vectors of new structures. The lattice constant of a Si (111) single crystal is known, and the value a thereof Si(111) About 0.384 nm. According to the real space lattice arrangement relationship, assume a SiTe2 Is SiTe 2 The relationship can be obtained: 3 xa SiTe2 ＝2√3ⅹa Si(111) . SiTe can be calculated according to the equation 2 Lattice constant a of SiTe2 SiTe of approximately 0.44nm, close to bulk material 2 Lattice constant (0.428 nm). The structure with a lattice period of 0.44nm corresponds to a three-dimensional periodic arrangement of silicon atoms on the surface of the substrate, such as a single layer of SiTe in FIG. 5 2 Is shown in the top view of the atomic structure model, and at the same time, from the side viewIt is seen that the single-layer SiTe2 is a sandwich-like layered structure of a stacked arrangement of tellurium-silicon-tellurium atoms, which also confirms that the present invention successfully achieves a two-dimensional atomic-scale crystalline thin film material.
The foregoing describes the general principles of the present application in conjunction with specific embodiments, however, it is noted that the advantages, effects, etc. mentioned in the present application are merely examples and are not limiting, and they should not be considered essential to the various embodiments of the present application. Furthermore, the foregoing disclosure of specific details is for the purpose of illustration and description and is not intended to be limiting, since the foregoing disclosure is not intended to be exhaustive or to limit the disclosure to the precise details disclosed.
As used herein, words such as "including," "comprising," "having," and the like are open-ended words that mean "including, but not limited to," and are used interchangeably herein. As used herein, the words "or" and "refer to, and are used interchangeably with, the word" and/or, "unless the context clearly dictates otherwise. The word "such as" is used herein to mean, and is used interchangeably with, the phrase "such as but not limited to".
The previous description of the disclosed aspects is provided to enable any person skilled in the art to make or use the present application. Various modifications to these aspects will be readily apparent to those skilled in the art, and the generic principles defined herein may be applied to other aspects without departing from the scope of the application. Thus, the present application is not intended to be limited to the aspects shown herein but is to be accorded the widest scope consistent with the principles and novel features disclosed herein.
The foregoing description has been presented for purposes of illustration and description. Furthermore, the description is not intended to limit embodiments of the application to the form disclosed herein. While a number of example aspects and embodiments have been discussed above, those of skill in the art will recognize certain variations, modifications, alterations, additions and sub-combinations thereof.
Claims (10)
1. A preparation method of a silicon ditelluride two-dimensional crystal material is characterized by comprising the following steps:
processing a single crystal substrate in a vacuum environment to obtain a reconstructed surface, wherein the single crystal substrate is a silicon single crystal; and
and evaporating and depositing tellurium atoms onto the single crystal substrate, and keeping the single crystal substrate at a set temperature so that tellurium and silicon react with each other to form a two-dimensional crystal material with a periodic structure.
2. The production method according to claim 1, wherein the processing of the single crystal substrate includes:
heating the single crystal substrate in vacuum at a heating rate of more than 400 ℃/s;
preserving the heat of the heated single crystal substrate for a preset time; and
the single crystal substrate is cooled to obtain a reconstituted surface.
3. The method of claim 1 or 2, wherein the reconstructed surface is a Si (111)7 x 7 structure.
4. The method as claimed in claim 1, wherein the set temperature is 350-400 ℃.
5. The method of claim 1, wherein the evaporation deposition is resistive heating evaporation deposition, electron beam evaporation deposition.
6. The method of claim 5, wherein the resistive heating evaporation deposition is performed as follows: the resistance wire is electrified and heated to ensure that the evaporation source is heated to a preset temperature to evaporate tellurium atoms, and the evaporated tellurium atoms form a beam to be deposited on the substrate.
7. The method of claim 6, wherein the deposition time is 5-20 minutes.
8. The method of any preceding claim, wherein the method further comprises: and slowly cooling the two-dimensional crystal material obtained after deposition to room temperature.
9. A silicon ditelluride two-dimensional crystal material is characterized in that crystal atoms are arranged in a triangular periodic manner and are orderly expanded in a two-dimensional plane to form a silicon ditelluride film material.
10. The method of claim 9, wherein the silicon ditelluride has a lattice period of 0.44nm, the lattice period being characterized by low energy electron diffraction.
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| CN115652260A (en) * | 2022-11-11 | 2023-01-31 | 湖南大学 | Preparation method of monatomic germanium and few-atom cluster |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN115652260A (en) * | 2022-11-11 | 2023-01-31 | 湖南大学 | Preparation method of monatomic germanium and few-atom cluster |
| CN115652260B (en) * | 2022-11-11 | 2023-05-16 | 湖南大学 | Preparation method of single-atom germanium and few-atom clusters |
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