Method for preparing rhenium disulfide film
By incorporating Re2O7 into soda-lime glass and introducing Na ions, the problem of rapid evaporation when Re2O7 is a rhenium source is solved, and the preparation of high-quality ReS2 films is achieved.
Patent Information
- Application Number
- CN202411892167.3
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2024-12-20
- Publication Date
- 2025-03-25
- Estimated Expiration
- Not applicable · inactive patent
AI Technical Summary
In the preparation of chemical vapor deposition method (CVD) of rhenium disulfide (ReS2) (CVD), when rhenium heptadecanoeutic (Re2O7) is used as the rhenium source, it is prone to evaporation, resulting in high nucleation density, forming particles instead of thin films, and there is a problem of controllability.
Re2O7 is incorporated into soda-lime glass as a rhenium source, and Na ions are introduced during the growth process, soda-lime glass slows down the evaporation rate of Re2O7 and promotes the formation of ReS2 film.
The rapid evaporation of Re2O7 is effectively avoided, the nucleation density of ReS2 is reduced, the lateral growth of crystal domains is promoted, and the formation of defects is inhibited, and high-quality ReS2 film is obtained.
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Figure CN119685792A_ABST
Abstract
Description
Technical Field
[0001] The invention belongs to the technical field of semiconductor material preparation, and in particular relates to a method for preparing a rhenium disulfide film. Background Art
[0002] Two-dimensional transition metal chalcogenides (TMDCs) are a class of layered materials that are connected by covalent bonds within the plane and interact with each other by van der Waals forces. Among the many two-dimensional TMDCs materials, rhenium disulfide (ReS 2 ) has an asymmetric crystal structure, and its in-plane anisotropic optical and electrical properties and excellent environmental stability make it have potential application value in fields such as polarization photodetection devices.
[0003] In ReS 2 In the preparation of chemical vapor deposition (CVD) of rhenium, rhenium source is a focus of current research. A good rhenium source needs to have high reactivity and moderate evaporation rate. Currently, the commonly used rhenium sources include mixtures of rhenium and tellurium, rhenium oxides, etc., but there are still some problems in controllability. For example, in the case of rhenium heptoxide (Re 2 O 7 ) as a rhenium source, although the reaction activity is high, Re 2 O 7 It is easy to evaporate, resulting in a large nucleation density, which easily forms particles rather than thin films. Therefore, the optimization of rhenium source is an important research topic in the preparation of ReS by CVD. 2 A key issue for ReS films 2 Thin films have important research significance in both basic research and practical applications. Summary of the invention
[0004] The purpose of the present invention is to provide a method for preparing ReS 2 Thin film method, Re 2 O 7 Incorporating soda-lime glass as a rhenium source, slowing down Re 2 O 7 The evaporation rate is high, and Na ions are introduced to assist in the growth process, on this basis, high-quality ReS 2 Thin films, further promoting their application in electrical devices.
[0005] The technical solution adopted by the present invention is as follows:
[0006] A method for preparing ReS 2 The method of the thin film comprises the following steps:
[0007] (1) Cleaning the graphite boat and substrate: The graphite boat, soda-lime glass and mica substrate were placed in acetone ultrasonic bath for 15 min, anhydrous ethanol for 15 min, and deionized water for 15 min, and then dried with a nitrogen gun.
[0008] (2) Weigh sulfur powder (S) with an electronic scale and feed it into the first temperature zone of the tube furnace; weigh Re with an electronic scale 2 O 7 Powder, weigh the Re 2 O 7 The powder is spread on the graphite boat, then covered with soda-lime glass, and then the mica substrate is placed on the soda-lime glass. Finally, the graphite boat is sent to the second temperature zone of the tube furnace. Under argon gas 100sccm, the first temperature zone and the second temperature zone are heated to 110℃ and kept warm for 10 minutes to remove water vapor. The schematic diagram of the device is shown in Figure 1 shown.
[0009] (3) Stop the argon gas, keep the temperature of the first temperature zone unchanged, raise the temperature of the second temperature zone to 750℃, and then keep it warm for a certain period of time to make Re 2 O 7 The powder is dissolved in the molten soda-lime glass; the schematic diagram of the device is as follows Figure 2 shown.
[0010] (4) In a certain argon atmosphere, the first temperature zone and the second temperature zone are heated to 150-350°C and 750-900°C respectively, and then kept at atmospheric pressure for a growth time to perform ReS 2 The film grows and finally cools naturally to room temperature to obtain ReS 2 Thin film; the schematic diagram of the device is as follows Figure 3 shown.
[0011] Furthermore, in step (2), the mass of S powder is 30-2000 mg.
[0012] Furthermore, in step (2), Re 2 O 7 The powder mass is 10-100 mg.
[0013] Furthermore, in step (3), the insulation time is 10-30 minutes.
[0014] Furthermore, in step (4), the argon gas flow rate is 10-200 sccm.
[0015] Furthermore, in step (4), the temperature in the first temperature zone is 150-350°C.
[0016] Furthermore, in step (4), the temperature of the second temperature zone is 750-900°C.
[0017] Furthermore, in step (4), the growth time is 5-60 min.
[0018] In summary, by adopting the above technical solution, the beneficial effects of the present invention are:
[0019] (1) In the present invention, in step (3), the first temperature zone is only 110°C, which means that sulfur does not evaporate to participate in the reaction; the temperature of the second temperature zone is 750°C, and the soda-lime glass becomes molten. Since Re2O7 is placed under the soda-lime glass, Re 2 O 7 Will be melted into the soda-lime glass and will not evaporate onto the upper mica substrate. 2 O 7 Melting into molten soda-lime glass as a rhenium source is beneficial to the ReS 2 All reactions take place in the molten soda-lime glass.
[0020] (2) In the present invention, in step (4), the first temperature zone and the second temperature zone are respectively raised to the growth temperature, sulfur is evaporated, driven by the carrier gas to the molten soda-lime glass, and reacts with Re under the catalysis of Na ions. 2 O 7 The reaction generates ReS in the molten soda-lime glass. 2 ; Then, ReS 2 It diffuses to the surface of the molten glass; finally, driven by the carrier gas, it is deposited on the mica substrate above to form a continuous film. 2 Synthesis reaction can effectively avoid Re 2 O 7 Rapid evaporation, thereby reducing the ReS 2 The nucleation density.
[0021] (3) In the present invention, in step (4), ReS 2 In the synthesis reaction, the presence of Na ions will effectively reduce the ReS 2 The formation of potential barriers promotes the lateral growth of crystal domains and inhibits the formation of defects, thereby forming high-quality films.
[0022] (4) In the present invention, ReS 2 The number of film layers can be determined by the Re 2 O 7 The quality and growth time in step (4) are controlled. BRIEF DESCRIPTION OF THE DRAWINGS
[0023] In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings required for use in the embodiments are briefly introduced below. It should be understood that the following drawings only show certain embodiments of the present invention and therefore should not be regarded as limiting the scope. For ordinary technicians in this field, other related drawings can be obtained based on these drawings without creative work.
[0024] Figure 1 The present invention is to prepare ReS 2 Schematic diagram of the film device.
[0025] Figure 2 The present invention is to prepare ReS 2 Schematic diagram of the film device.
[0026] Figure 3 The present invention is to prepare ReS 2 Schematic diagram of the film device. DETAILED DESCRIPTION
[0027] In order to make the purpose, technical scheme and advantages of the present invention more clearly understood, the present invention is further described in detail below in conjunction with the accompanying drawings and embodiments. It should be understood that the specific embodiments described herein are only used to explain the present invention and are not used to limit the present invention, that is, the embodiments described are only part of the embodiments of the present invention, rather than all of the embodiments. The components of the embodiments of the present invention described and shown in the drawings herein can be arranged and designed in various different configurations.
[0028] Therefore, the following detailed description of the embodiments of the present invention provided in the accompanying drawings is not intended to limit the scope of the invention claimed for protection, but merely represents selected embodiments of the present invention. Based on the embodiments of the present invention, all other embodiments obtained by those skilled in the art without making creative work are within the scope of protection of the present invention.
[0029] It should be noted that relational terms such as "first" and "second" are used only to distinguish one entity or operation from another entity or operation, and do not necessarily require or imply any such actual relationship or order between these entities or operations. Moreover, the terms "include", "comprise" or any other variants thereof are intended to cover non-exclusive inclusion, so that a process, method, article or device including a series of elements includes not only those elements, but also other elements not explicitly listed, or also includes elements inherent to such process, method, article or device. In the absence of further restrictions, the elements defined by the sentence "comprise a ..." do not exclude the existence of other identical elements in the process, method, article or device including the elements.
[0030] The features and performance of the present invention are further described in detail below in conjunction with the embodiments.
[0031] Example 1
[0032] (1) Cleaning the graphite boat and substrate: Separately clean the graphite boat, ~1×1 cm 2The soda-lime glass and mica substrates were placed in acetone ultrasound for 15 min, anhydrous ethanol for 15 min, deionized water for 15 min, and dried with a nitrogen gun.
[0033] 2) Weigh 200 mg of S powder with an electronic scale and send it into the first temperature zone of the tube furnace; weigh Re with an electronic scale 2 O 7 5mg, weigh Re 2 O 7 The powder is spread on the graphite boat, then covered with soda-lime glass, and then the mica substrate is placed on the soda-lime glass. Finally, the graphite boat is sent to the second temperature zone of the tube furnace. Under argon gas 100sccm, the first temperature zone and the second temperature zone are heated to 110℃ and kept warm for 10 minutes to remove water vapor. The schematic diagram of the device is shown in Figure 1 shown.
[0034] (3) Stop the argon gas, keep the temperature of the first temperature zone unchanged, raise the temperature of the second temperature zone to 750°C, and then keep it at this temperature for 20 minutes under argon gas of 10 sccm. 2 O 7 The powder is dissolved in the molten soda-lime glass; the schematic diagram of the device is as follows Figure 2 shown.
[0035] (4) Under argon gas at 30 sccm, the first temperature zone and the second temperature zone were heated to 250°C and 800°C, respectively, and then kept at atmospheric pressure for 20 min to perform ReS 2 The film grows and finally cools naturally to room temperature to obtain a single layer of ReS 2 Thin film; the schematic diagram of the device is as follows Figure 3 shown.
[0036] The above description is only a preferred embodiment of the present invention and is not intended to limit the present invention. Any modifications, equivalent substitutions and improvements made within the spirit and principles of the present invention should be included in the protection scope of the present invention.
Claims
1. A method for preparing a rhenium disulfide (ReS2) thin film, comprising the following steps: (1) Cleaning the graphite boat and substrate: The graphite boat, soda-lime glass and mica substrate were placed in acetone ultrasonic bath for 15 min, anhydrous ethanol for 15 min, and deionized water for 15 min, and then dried with a nitrogen gun. (2) Weigh sulfur powder (S) with an electronic scale and place it in the first temperature zone of the tube furnace; weigh rhenium heptoxide (Re2O7) powder with an electronic scale, spread the weighed Re2O7 powder on a graphite boat, then cover it with soda-lime glass, then place a mica substrate on top of the soda-lime glass, and finally place the graphite boat into the second temperature zone of the tube furnace; raise the temperature of the first and second temperature zones to 110°C under argon gas at 100 sccm, keep them warm for 10 min, and remove water vapor; the schematic diagram of the device is shown in FIG1 . (3) Stop the argon gas, keep the temperature of the first temperature zone unchanged, raise the temperature of the second temperature zone to 750°C, and then keep it at this temperature for a certain period of time to dissolve the Re2O7 powder in the molten soda-lime glass; the schematic diagram of the device is shown in FIG2. (4) Under a certain argon atmosphere, the first temperature zone and the second temperature zone are heated to 150-350°C and 750-900°C respectively, and then kept at atmospheric pressure for a growth time to grow the ReS2 thin film, and finally naturally cooled to room temperature to obtain the ReS2 thin film; the schematic diagram of the device is shown in FIG3 .
2. A method for preparing a ReS2 thin film according to claim 1, characterized in that: In step (3), the first temperature zone is only 110°C, which means that sulfur does not evaporate to participate in the reaction; the temperature of the second temperature zone is 750°C, and the soda-lime glass becomes molten. Since Re2O7 is placed under the soda-lime glass, Re2O7 will melt into the soda-lime glass and will not evaporate onto the mica substrate above. Re2O7 is melted into the molten soda-lime glass as a rhenium source, which is beneficial to the reaction of ReS2 in step (4) to occur in the molten soda-lime glass.
3. A method for preparing a ReS2 thin film according to claim 1, characterized in that: In step (4), the first temperature zone and the second temperature zone are respectively raised to the growth temperature, sulfur is evaporated, and driven by the carrier gas to the molten soda-lime glass, and reacts with Re2O7 under the catalysis of Na ions to generate ReS2 inside the molten soda-lime glass; then, ReS2 diffuses to the surface of the molten glass; finally, driven by the carrier gas, it is deposited on the mica substrate above to form a continuous film. The ReS2 synthesis reaction occurs in the molten soda-lime glass, which can effectively avoid the rapid evaporation of Re2O7, thereby reducing the nucleation density of ReS2.
4. A method for preparing a ReS2 thin film according to claim 1, characterized in that: In step (4), a ReS2 synthesis reaction occurs in the molten soda-lime glass. The presence of Na ions will effectively reduce the formation barrier of ReS2, thereby promoting the lateral growth of crystal domains and inhibiting the formation of defects, thereby forming a high-quality film.
5. A method for preparing a ReS2 thin film according to claim 1, characterized in that: The number of layers of the ReS2 film can be controlled by the quality of Re2O7 in step (2) and the growth time in step (4).