A method for preparing zirconium pentatelluride thin film

Abstract

The present invention discloses a method for preparing a zirconium pentatelluride thin film, specifically comprising the following steps: first, growing ZrTe5 crystals using a flux method, grinding them into powder, and adding a dispersant for intercalation treatment to weaken the van der Waals forces between the ZrTe5 crystal layers; then, using ultrasonic dispersion technology, preparing a ZrTe5 dispersion with good dispersibility. To improve the stability of the dispersion, a stabilizer is further added to significantly enhance the dispersion and stability of the ZrTe5 particles in the solution. Finally, a uniform thin film is deposited by spin coating or drop coating. The method of the present invention is simple to operate, low-cost, and suitable for the preparation and application of topological functional materials.

Description

Technical Field

[0001] The invention relates to the technical field of nano material preparation and describes a method for preparing a zirconium pentatelluride film. Background Art

[0002] Topological materials are currently a frontier research topic attracting widespread attention in condensed matter physics and materials science. Unlike traditional materials, topological materials exhibit bulk insulation and boundary state conductivity due to strong spin-orbit coupling. This novel electronic topological property holds great potential for applications in spintronics, quantum computing, and low-power electronic devices. With the miniaturization of electronic devices, research on two-dimensional topological materials is increasing. Two-dimensional topological materials possess unique properties, such as one-dimensional topological boundary states and the quantum spin Hall effect, which give them enhanced stability, integration, and unique application potential in dissipative electron transport and nanoelectronics. As a star material among two-dimensional topological materials, ZrTe5 has attracted considerable attention due to its combination of topological insulator, thermoelectric, and quantum transport properties.

[0003] The energy gap characteristics of ZrTe5 are complex and variable, significantly affected by factors such as crystal structure, temperature, and pressure. At room temperature, ZrTe5 is a narrow-bandgap semiconductor with high mid-infrared light absorption and excellent thermoelectric properties, showing broad application prospects in optoelectronic devices, flexible thermoelectric materials, and wearable power generation or temperature sensing. At low temperatures, as the energy gap approaches zero and even band overlap occurs, ZrTe5 transforms into a topological Dirac semimetal with extremely high electron mobility, significant spin-orbit coupling, and quantum transport properties, making it suitable for the development of quantum computing, high-performance sensors, and topological electronic devices. In addition, ZrTe5's dynamic control capabilities enable flexible switching of electronic states under external stimuli (such as pressure and magnetic fields), further expanding its functional applications. Its excellent physical and chemical properties make ZrTe5 a research focus for new functional materials.

[0004] Currently, ZrTe5 thin films are primarily prepared by mechanical exfoliation. Although this method is simple and inexpensive, it is difficult to produce large-scale films with uniform thickness at the millimeter level due to the quasi-one-dimensional linear and strip-like structure of ZrTe5. Therefore, large-scale preparation of highly crystalline ZrTe5 thin films is an urgent problem.

[0005] Therefore, preparing topological material dispersions based on a solution method has become a viable alternative. By depositing a uniformly dispersed topological material dispersion on a substrate, thin films with few surface defects and a uniform and dense structure can be obtained. Currently, the main methods for preparing topological material dispersions include liquid phase dispersion, chemical dispersion, electrochemical dispersion, and mechanical ball milling. Among them, liquid phase dispersion is the preferred method for preparing topological material dispersions due to its simplicity, low cost, and high efficiency. Liquid phase dispersion can produce topological material dispersions with high crystallinity, few defects, and excellent electrical properties. Thin films prepared using such dispersions show broad application prospects in flexible electronic devices, optoelectronic devices, sensors, and energy storage and conversion. However, ZrTe5 particles have poor stability during solution dispersion, making it difficult to achieve highly uniform thin films. Summary of the Invention

[0006] The purpose of the present invention is to prepare a stable ZrTe5 dispersion using a liquid-phase ultrasonic dispersion technology with a simple operation process and low cost, and further achieve uniform thin film deposition by a spin coating or drop coating method.

[0007] The specific technical solution for achieving the purpose of the present invention is:

[0008] A method for preparing a zirconium pentatelluride thin film comprises the following specific steps:

[0009] (1) Growth of ZrTe5 crystals: Zr and Te powders are placed in a quartz tube at a molar ratio of 1:45-50 and sealed in a vacuum chamber. The tube is then placed in a muffle furnace at a set temperature of 950-1100 °C for 20-30 h to allow the mixture to fully melt and form a uniform Zr-Te melt. The temperature is then lowered in two stages: the first stage is rapid cooling at 600-650 °C; the second stage is slow cooling at 450-500 °C until the crystal growth is complete.

[0010] (2) preparing a ZrTe5 dispersion: crushing the ZrTe5 crystals grown in step (1) into powder in an agate mortar; placing the ZrTe5 powder in a container, adding a dispersant and mixing uniformly; placing the mixture in an ultrasonic processor to achieve dispersion to obtain a ZrTe5 dispersion, and then adding a stabilizer to the dispersion to fully mix it; wherein the dispersant is selected from one or more of 1-pyrenesulfonic acid sodium salt, 2-hydroxy-7-naphthalenesulfonic acid sodium salt, dimethyl sulfoxide, N-methylpyrrolidone and N,N-dimethylformamide; when using 1-pyrenesulfonic acid sodium salt or 2-hydroxy-7-naphthalenesulfonic acid sodium salt as a dispersant, deionized water should be added as a solvent; ZrTe5, 1-pyrenesulfonic acid sodium salt or 2-hydroxy-7-naphthalenesulfonic acid sodium salt and deionized water are prepared according to 5 mg: 1 ~ 2 mg: 1 ~ 2 mL; using dimethyl sulfoxide, N-methylpyrrolidone or N When N-dimethylformamide is used as a dispersant, the concentration of the ZrTe5 dispersion is 1-10 mg / mL; the stabilizer is terpineol or oleylamine, wherein the volume ratio of the ZrTe5 dispersion to the stabilizer is 10:1; the ultrasonic power is 100-120 W, and the ultrasonic temperature is maintained at 20-40°C;

[0011] (3) Preparing a ZrTe5 thin film: The ZrTe5 dispersion prepared in step (2) is applied to a substrate by spin coating or drop coating to form a ZrTe5 thin film, which is then vacuum annealed and cooled to room temperature to obtain the zirconium pentatelluride thin film; the vacuum annealing temperature is 60-120°C and the annealing time is 5-30 min.

[0012] Furthermore, the substrate is a silicon / silicon dioxide substrate, an aluminum oxide substrate or a conductive glass; wherein the substrate is cleaned with deionized water, acetone and isopropyl alcohol before spin coating or drop coating.

[0013] A zirconium pentatelluride film prepared based on the above method.

[0014] The invention prepares ZrTe5 dispersion liquid based on liquid phase ultrasonic dispersion technology, has simple preparation process and low cost; the prepared thin film has high crystallinity, relatively few defects and good electrical properties.

[0015] In addition, the two-dimensional ZrTe5 particles after ultrasonic dispersion have a very high specific surface area. The van der Waals forces between the layers make the ZrTe5 particles in the dispersion liquid prone to sedimentation and agglomeration, and the prepared ZrTe5 dispersion is unstable. In the present invention, the dispersion degree of the ZrTe5 dispersion is adjusted by adding a stabilizer, so that it has good dispersibility and is not prone to agglomeration or sedimentation. At the same time, the uniformity of the thin film deposition is significantly improved, and high-quality ZrTe5 thin films can be prepared directly on the substrate using spin coating or drop coating processes. In addition, by adjusting the spin coating speed and time, the thickness of the ZrTe5 thin film can also be precisely controlled, thus laying a solid foundation for its application in electronic devices and related fields. BRIEF DESCRIPTION OF THE DRAWINGS

[0016] Figure 1 is a flow chart of the present invention;

[0017] Figure 2 Schematic diagram of the ZrTe5 dispersion prepared in the present invention;

[0018] Figure 3 These are optical microscope images of the ZrTe5 thin film obtained in Example 1 of the present invention under different magnifications. DETAILED DESCRIPTION

[0019] The present invention provides a method for preparing a zirconium pentatelluride thin film. To clarify the objectives, technical solutions, and advantages of the present invention, the present invention is described in more detail below. It should be noted that the specific embodiments described herein are intended only to illustrate and explain the present invention and are not intended to limit the scope of the present invention.

[0020] The present invention uses liquid-phase ultrasonic dispersion technology to prepare a stable ZrTe5 dispersion by adding a suitable dispersant, resulting in a simple and low-cost process. Furthermore, the use of a suitable stabilizer improves the dispersion and stability of the ZrTe5 particles in the dispersion, enabling uniform thin-film deposition via spin coating or drop coating.

[0021] The present invention provides the following examples to provide a more complete understanding of the present invention.

[0022] The ZrTe5 crystals described in the following examples were all prepared using the following co-solvent method. Zr and Te elemental powders were placed in a quartz tube at a molar ratio of 1:45-50 and vacuum-sealed. The tube was then placed in a muffle furnace at a set temperature of 950-1100°C for 20-30 hours to allow the mixture to fully melt and form a uniform Zr-Te melt. The temperature was then lowered in two stages: the first stage was rapid cooling at 600-650°C; the second stage was slow cooling at 450-500°C until the crystal growth was complete. Figure 1 shown. Example

[0023] Take 10 mg of flux-grown ZrTe5 crystals and grind them into powder using an agate mortar. Add the ZrTe5 powder and 2 mL of N-methylpyrrolidone into a container. Set the ultrasonic processor to 30 °C and 120 W to sonicate the solution for 4 hours to obtain a ZrTe5 dispersion. Then add 200 μL of oleylamine and stir in a magnetic stirrer for 5 minutes. Figure 2 shown.

[0024] The silicon / silicon dioxide substrate was 1 cm × 1 cm in size and was cut manually using a scriber. It was cleaned with deionized water, acetone, and isopropanol before spin coating. The ZrTe5 dispersion was then spun at a low speed of 300 rpm for 20 s and vacuum annealed at 120 °C for 20 min. The resulting ZrTe5 film was as shown in Figure 2. Figure 3 Shown are optical microscope images of ZrTe5 topological thin films under different magnifications (scale: 0.1 mm). Example

[0025] Grind 10 mg of flux-grown ZrTe5 crystals into a powder using an agate mortar. Add the ZrTe5 powder and 5 mL of N,N-dimethylformamide to a container. Ultrasonicate the solution at 25°C and 100 W power for 8 hours to obtain a ZrTe5 dispersion. Add 500 μL of oleylamine as a stabilizer and stir in a magnetic stirrer for 10 minutes.

[0026] Silicon / silicon dioxide substrates (alumina substrates, conductive glass substrates) were all 1 cm × 1 cm and were cut manually using a scriber. Before spin coating, they were cleaned with deionized water, acetone, and isopropyl alcohol. The dispersion was then spin-coated onto the chip at a constant speed of 500 rpm and annealed in a vacuum at 120°C for 20 minutes. Example

[0027] 5 mg of flux-grown ZrTe5 crystals were ground into powder using an agate mortar. The ZrTe5 powder was added to a container along with 2 mL of dimethyl sulfoxide (DMSO). The solution was sonicated for 6 hours using an ultrasonic processor set at 20°C and 120 W power to obtain a ZrTe5 dispersion. 200 μL of terpineol was added as a stabilizer, and the mixture was stirred in a magnetic stirrer for 15 minutes.

[0028] Both the silicon / silicon dioxide and alumina substrates were 1 cm × 1 cm in size and were cut manually using a scriber. Before spin coating, they were pre-cleaned with deionized water, acetone, and isopropyl alcohol. An appropriate amount of ZrTe5 dispersion was then dropped onto the silicon / silicon dioxide (or alumina) substrate using a pipette, dried at room temperature for 20 minutes, and finally annealed in a vacuum at 60°C for 25 minutes. Example

[0029] 5 mg of flux-grown ZrTe5 crystals were ground into powder using an agate mortar. The ZrTe5 powder, 1 mL of deionized water, and 2 mg of 1-pyrenesulfonic acid sodium salt were added to a container. The solution was sonicated for 10 hours at a power of 120 W and a temperature of 35°C to obtain a ZrTe5 dispersion. 100 μL of oleylamine was then added as a stabilizer, and the mixture was stirred in a magnetic stirrer for 5 minutes.

[0030] Conductive glass sheets were cut manually to 1 cm × 1 cm using a scriber. They were pre-cleaned with deionized water, acetone, and isopropyl alcohol before spin coating. The dispersion was then spin-coated onto the conductive glass at a constant speed of 800 rpm and annealed in a vacuum at 90°C for 30 min.

Claims

1. A method for preparing a zirconium pentatelluride thin film, characterized in that: The steps include: (1) Growth of ZrTe5 crystals: Zr and Te powders are placed in a quartz tube at a molar ratio of 1:45-50 and sealed in a vacuum chamber. The tube is then placed in a muffle furnace at a set temperature of 950-1100 °C for 20-30 h to allow the mixture to fully melt and form a uniform Zr-Te melt. The temperature is then lowered in two stages: the first stage is rapid cooling at 600-650 °C; the second stage is slow cooling at 450-500 °C until the crystal growth is complete. (2) preparing a ZrTe5 dispersion: crushing the ZrTe5 crystals grown in step (1) into powder in an agate mortar; placing the ZrTe5 powder in a container, adding a dispersant and mixing uniformly; placing the mixture in an ultrasonic processor to achieve dispersion to obtain a ZrTe5 dispersion, and then adding a stabilizer to the dispersion to fully mix it; wherein the dispersant is selected from one or more of 1-pyrenesulfonic acid sodium salt, 2-hydroxy-7-naphthalenesulfonic acid sodium salt, dimethyl sulfoxide, N-methylpyrrolidone and N,N-dimethylformamide; when using 1-pyrenesulfonic acid sodium salt or 2-hydroxy-7-naphthalenesulfonic acid sodium salt as a dispersant, deionized water should be added as a solvent; ZrTe5, 1-pyrenesulfonic acid sodium salt or 2-hydroxy-7-naphthalenesulfonic acid sodium salt and deionized water are prepared according to 5 mg: 1 ~ 2 mg: 1 ~ 2 mL; using dimethyl sulfoxide, N-methylpyrrolidone or N When N-dimethylformamide is used as a dispersant, the concentration of the ZrTe5 dispersion is 1-10 mg / mL; the stabilizer is terpineol or oleylamine, wherein the volume ratio of the ZrTe5 dispersion to the stabilizer is 10:1; the ultrasonic power is 100-120 W, and the ultrasonic temperature is maintained at 20-40°C; (3) Preparing a ZrTe5 thin film: The ZrTe5 dispersion prepared in step (2) is applied to a substrate by spin coating or drop coating to form a ZrTe5 thin film, which is then subjected to vacuum annealing and cooled to room temperature to obtain the zirconium pentatelluride thin film; the vacuum annealing temperature is 60-120°C and the annealing time is 5-30 min.

2. The method for preparing a zirconium pentatelluride thin film according to claim 1, wherein: The substrate is a silicon / silicon dioxide substrate, an aluminum oxide substrate or a conductive glass; wherein the substrate is cleaned with deionized water, acetone and isopropyl alcohol before spin coating or drop coating.

3. A zirconium pentatelluride thin film prepared based on the method according to claim 1.

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