CN-121974694-A - Two-dimensional transition metal chalcogenide target and preparation method thereof

Abstract

The invention relates to the technical field of functional material preparation, in particular to a two-dimensional transition metal chalcogenide target and a preparation method thereof. The method comprises the steps of mixing high-purity tellurium and transition metal, carrying out vacuum swing smelting on the transition metal which is high-purity tungsten or high-purity molybdenum at 1100-1300 ℃ to obtain cast ingots, crushing and ball-milling the cast ingots to obtain micron-sized powder, carrying out high-energy ball milling on the micron-sized powder to obtain nanometer-sized powder, carrying out heat treatment on the nanometer-sized powder at 150-160 ℃ to obtain heat-treated nanometer powder, carrying out presintering on the heat-treated nanometer powder at 300-400 ℃, carrying out high-temperature sintering at 500-750 ℃ and 20-40 MPa to obtain target blanks, and carrying out hot isostatic pressing treatment on the target blanks at 500-650 ℃ and 80-150 MPa. The preparation method provided by the invention can obtain the high-quality alloy target material with high density, large size and uniform components.

Inventors

• LIU XIU
• YANG PENG
• JIANG CHUANNING
• HE JINJIANG
• Ran Yutong
• DING ZHAOCHONG
• JIA QIAN
• Hua Yongle
• LIN XINYU

Assignees

• 有研亿金新材料有限公司
• 有研亿金新材料(山东)有限公司

Dates

Publication Date

20260505

Application Date

20260409

Claims (10)

1. 1. The preparation method of the two-dimensional transition metal chalcogenide target is characterized by comprising the following steps of: 1) Mixing high-purity tellurium and transition metal, wherein the transition metal is high-purity tungsten or high-purity molybdenum, and carrying out vacuum swing smelting at 1100-1300 ℃ to obtain an ingot; 2) Crushing and ball milling the cast ingot to obtain micron-sized powder: 3) Performing high-energy ball milling on the micron-sized powder to obtain nano-sized powder; 4) Heat-treating the nanoscale powder at 150-200 ℃ to obtain heat-treated nanoscale powder; 5) Presintering the heat-treated nano powder at 300-400 ℃, and then sintering at high temperature of 500-750 ℃ and 20-40 MPa ℃ to obtain a target blank; 6) The target blank is hot isostatic pressed at 500-650 ℃ and 80-150 MPa.
2. 2. The method according to claim 1, wherein in step 1), the vacuum swing smelting is performed for 8-12 hours, the swing frequency is 10-15 times/min, and the heating rate is 70-90 ℃.
3. 3. The preparation method according to claim 1, wherein in the step 2), the ball milling tank and the ball milling balls are made of W or Mo, the D50 particle size of the micron-sized powder is 30-100 μm, the ball milling rotating speed is 400-600 r/min, and the ball milling time is 40-90min.
4. 4. The method according to claim 3, wherein in the step 3), the D90 particle diameter of the nano-sized powder is not more than 100nm.
5. 5. The method according to any one of claims 1 to 4, wherein in step 4), the nano-sized powder is subjected to air classification to obtain a target particle size powder having a particle size of 50 to 90nm, and heat-treated under an argon atmosphere at 150 to 200 ℃ for 90 to 120 minutes.
6. 6. The method according to any one of claims 1 to 4, wherein in step 5), the pre-sintering time is 1 to 2 hours and the high-temperature sintering time is 1 to 3 hours.
7. 7. The method according to any one of claims 1 to 4, wherein in step 6), the hot isostatic pressing is performed for a period of 2 to 3 hours.
8. 8. The method of any one of claims 1-4, further comprising step 7) of machining, buffing and welding the backing plate to the densified target blank from step 6).
9. 9. A two-dimensional transition metal chalcogenide target material, characterized in that it is prepared by the preparation method according to any one of claims 1 to 8.
10. 10. The two-dimensional transition metal chalcogenide target according to claim 9, wherein the density of the target is not less than 99%, the purity is not less than 99.995%, the diameter is not less than 400 mm, the thickness is 5-12 mm, and the component deviation is not more than 0.5 at%.

Description

Two-dimensional transition metal chalcogenide target and preparation method thereof Technical Field The invention relates to the technical field of functional material preparation, in particular to a two-dimensional transition metal chalcogenide target and a preparation method thereof. Background The two-dimensional transition metal chalcogenide (TMDs) has broad application prospects in the fields of electronic devices, photoelectric devices, energy storage and the like due to unique electronic structures, lamellar characteristics and controllable energy band structures. The WTE 2 and MoTe 2 are taken as typical TMDs materials, have excellent electrical, optical and thermal properties, and are suitable for high-performance transistors, memories, sensors, neuromorphic devices and the like. WTe 2 has the properties of unsaturated giant magnetoresistance, narrow bandgap, superconductivity at high voltage, etc., and can be applied to field effect transistors and energy storage devices, and is considered to be a second type of Weyl half-metal. MoTe 2 has excellent photoelectric characteristics, low heat conductivity and other properties, and can be applied to the fields of photoelectric devices, thermoelectric materials and the like. Currently, the methods for preparing WTe 2 and MoTe 2 films mainly comprise mechanical stripping, chemical Vapor Deposition (CVD), chemical Vapor Transport (CVT), pulsed Laser Deposition (PLD), and the like. PLD technology is an important means for preparing high-quality TMDs films because of the advantages of low-temperature deposition, high component fidelity, suitability for various substrates and the like. However, the PLD process has extremely high quality requirements on the target material, and needs to have the characteristics of high purity, high density, component uniformity, large size and the like. In the prior art, methods for preparing WTE 2 and MoTe 2 targets are rarely reported. Because of the large difference between the melting point of W, mo and Te (W: 3422℃, mo:2623℃, te:449.5 ℃), te is easy to volatilize during smelting and high-temperature sintering, so that component segregation is caused, and a large-size target with uniform components and high density is difficult to obtain. For example, CN120015704a has advantages in the preparation of small-area, high-cleanliness corner two-dimensional materials, but is limited by material type, process complexity, equipment dependence, and scale challenges. Practical application is required to balance these limitations according to specific requirements. CN119220953a is only suitable for tellurium powder, tungsten trioxide and potassium bromide as precursors, and other materials need to be compatible for verification. The method has advantages only in the preparation of small-size and high-quality single-layer films, but has limitations in the aspects of large-area uniform growth, stability of process parameters and material universality, and needs to be further optimized to meet the industrial requirements. CN120591884a needs to strictly control the stoichiometric ratio of molybdenum powder, tellurium powder and cobalt powder, and the deviation may cause the quality degradation of the product. The method has remarkable results in terms of simplifying the flow and improving the efficiency, but is limited by factors such as raw material purity, equipment dependence, process parameter sensitivity and the like, and the bottleneck of the traditional method is not completely broken through. The commercial application of the method still needs to solve the problems of large-scale production, cost control, product performance optimization and the like. CN119800498a successfully prepares a WTe 2 film with high quality, and demonstrates the advantages of the WTe 2 film in terms of improving the coverage, continuity and uniformity of the film, but the problems of complex preparation process, high requirements on materials and equipment, strong dependence on film quality, expandability, challenges in mass production and the like still exist. To realize the practical application of the method, the process is further optimized, the cost is reduced, the expansibility and the large-scale production capacity are improved, and the performance of the film is more comprehensively estimated and verified. Therefore, developing a method for preparing a high-quality WTE 2/MoTe2 target material suitable for PLD technology has important industrial application value. Disclosure of Invention In order to solve the technical problems, the invention provides a two-dimensional transition metal chalcogenide target and a preparation method thereof. The invention is based on a powder metallurgy process to prepare a two-dimensional transition metal chalcogenide (TMDs) target for Pulse Laser Deposition (PLD), in particular to a tungsten ditelluride (WTE 2) and molybdenum ditelluride (MoTe 2) target, which effectively solves the problems of uneven components