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CN-122012976-A - Tantalum-tungsten-based nano composite target material and preparation method thereof

CN122012976ACN 122012976 ACN122012976 ACN 122012976ACN-122012976-A

Abstract

The invention relates to the technical field of metal material preparation, in particular to a tantalum-tungsten-based nano composite target and a preparation method thereof. The method comprises the steps of smelting a high-purity tantalum block and a high-purity tungsten block, casting to obtain a tantalum-tungsten pre-alloy cast ingot, atomizing the tantalum-tungsten pre-alloy cast ingot to obtain Ta-W alloy powder, mixing the Ta-W alloy powder with a nano carbon material to obtain TaW-C mixed powder, performing magnetic field assisted sintering on the TaW-C mixed powder to induce grain directional growth, and performing aftertreatment to obtain the tantalum-tungsten-based nano composite target, wherein the magnetic field assisted sintering adopts a unidirectional static magnetic field along the direction of a vertical target surface, and the magnetic field strength is 2-10T. The invention can prepare the Ta-W based nano composite target material with high density, uniform tissue and texture orientation, and the deposited film has the characteristics of low stress, high flexibility and the like, thereby meeting the use requirement of the flexible implantation electrode.

Inventors

  • Ran Yutong
  • DING ZHAOCHONG
  • LI XINRAN
  • Shu Ruixi
  • HE JINJIANG
  • REN ZEHUA
  • JIA QIAN
  • FAN NING
  • LIN XINYU
  • Hua Yongle

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
20260512
Application Date
20260413

Claims (10)

  1. 1. The preparation method of the tantalum-tungsten-based nano composite target material is characterized by comprising the following steps: 1) Smelting a high-purity tantalum block and a high-purity tungsten block, and casting to obtain a tantalum-tungsten prealloy cast ingot; 2) Atomizing the tantalum-tungsten pre-alloy cast ingot to prepare powder to obtain Ta-W alloy powder; 3) Mixing the Ta-W alloy powder with a nano carbon material to obtain TaW-C mixed powder; 4) And performing magnetic field assisted sintering on the TaW-C mixed powder to induce grain directional growth, and performing post-treatment to obtain the tantalum-tungsten-based nano composite target, wherein the magnetic field assisted sintering adopts a unidirectional static magnetic field along the direction vertical to the target surface, and the magnetic field strength is 2-10T.
  2. 2. The preparation method according to claim 1, wherein in the step 1), the mass content of tungsten element in the tantalum-tungsten pre-alloy cast ingot is less than or equal to 12%.
  3. 3. The preparation method according to claim 1, wherein in the step 1), the smelting temperature is 2000-2500 ℃, the time is 10-100 min, and the vacuum degree is less than or equal to 10 -3 Pa; And/or, the smelting is vacuum induction smelting, vacuum consumable arc smelting or electron beam smelting; and/or the tantalum-tungsten pre-alloy cast ingot is cylindrical, and the diameter of the cast ingot is 20-80 mm.
  4. 4. The method according to any one of claims 1 to 3, wherein in the step 2), the atomization powder is plasma rotary electrode atomization or high-pressure gas atomization, and the particle diameter D50 of the Ta-W alloy powder is 50-150 μm; And/or, in the Ta-W alloy powder, the mass fraction of the powder with the particle size of 50-150 mu m is not less than 90%, and the oxygen content of the powder is less than or equal to 1000ppm.
  5. 5. The preparation method according to any one of claims 1 to 3, wherein in the step 3), the nano carbon material comprises one or more of amorphous carbon powder, multi-wall carbon nanotubes and graphene, wherein the particle size of the amorphous carbon powder is 0-200 nm, the outer diameter of the multi-wall carbon nanotubes is 5-50 nm, the length of the multi-wall carbon nanotubes is 0.5-5 μm, the thickness of the graphene is 1-20 nm, and the sheet diameter of the graphene is 0.5-5 μm; And/or mixing the nano carbon material with Ta-W alloy powder and performing ball milling, wherein the mass of the nano carbon material accounts for 0.01% -1.0% of the mass of the Ta-W alloy powder, absolute ethyl alcohol is used as a dispersion medium, the ball powder ratio is 5-15:1, the ball milling time is 1-6 hours, and the planetary ball mill is adopted for ball milling, and the ball milling rotating speed is 200-300 rpm.
  6. 6. The method according to claim 5, wherein in the step 3), the surface modification or coating treatment is further performed on the nano carbon material, and the ceramic material layer is coated on the surface of the nano carbon material by chemical vapor deposition or atomic layer deposition, wherein the ceramic material layer is boron nitride.
  7. 7. The method according to any one of claims 1 to 3, wherein in step 4), the sintering temperature is 1000 to 1500 ℃ and the pressure is 25 to 35mpa; And/or the sintering heat preservation time is 1-6 h, the heating rate is 10-100 ℃ per minute, and the sintering is performed in a vacuum environment of less than or equal to 10 -2 Pa or in a protective atmosphere.
  8. 8. The method according to claim 7, wherein in step 4), the sintering further comprises a medium-temperature vacuum annealing treatment of the obtained target blank, wherein the annealing temperature is 800-1000 ℃ and the annealing time is 1-4 hours.
  9. 9. The tantalum-tungsten-based nanocomposite target obtained by the production method according to any one of claims 1 to 8.
  10. 10. The tantalum-tungsten-based nanocomposite target according to claim 9, wherein the relative density of the tantalum-tungsten-based nanocomposite target is 99% -100%, the enhancement coefficient of the (001) crystal face texture strength in the direction perpendicular to the target surface is not less than 2% relative to the random polycrystal, and the tungsten content deviation in the tantalum-tungsten-based nanocomposite target is not more than 3%.

Description

Tantalum-tungsten-based nano composite target material and preparation method thereof Technical Field The invention relates to the technical field of metal material preparation, in particular to a tantalum-tungsten-based nano composite target and a preparation method thereof. Background Tantalum-tungsten alloy is used as a metal material with high strength, corrosion resistance and good biocompatibility and is applied to medical implantation devices such as cardiovascular stents and the like. In recent years, in the fields of flexible electronics, biosensing and the like, new application requirements are put forward on the tantalum-tungsten material, and particularly in the brain-computer interface flexible electrode, the tantalum-tungsten material serving as a conductive film layer is required to simultaneously meet the rigorous requirements of softness, flexibility, low internal stress, stable conductivity and the like. However, ta-W targets prepared by conventional processes are mainly used for hard electronic devices, such as integrated circuit interconnect layers, diffusion barrier layers, and the like, and often focus on high purity of materials, grain refinement, composition and structure uniformity, and improvement of sputtering rate and film thickness uniformity. For example, the invention patent application CN119489150A and the like adopts different technological means such as forging, rolling, additive manufacturing and the like, so that the performance improvement of the Ta-W alloy is realized. The invention patent application CN119328162A constructs a Ta-10W prealloy powder and high-purity Ta powder which are mixed in proportion and then are formed by laser selective melting, and then the Ta-W alloy which can be accurately regulated and controlled within the component range of 0-10 wt.% W and has compact structure and few defects is realized by a short-process preparation method of high-vacuum stress-relief heat treatment, the tensile strength of the obtained material reaches 550-726 MPa, the extensibility reaches 29-40%, and the traditional ingot forging process flow is obviously shortened. However, most of the methods aim at Ta-W films on rigid substrates, and new problems can occur when the Ta-W films are used on flexible polymer substrates, namely, the Ta-W films are easy to crack and delaminate under repeated bending with small curvature due to high hardness and large stress, so that the device is invalid. And, adding carbon nanomaterials to metal matrix composites presents challenges. The introduction of nanocarbon such as Carbon Nanotubes (CNT) into a metal matrix can improve strength and new properties, but also has problems of uneven dispersion and interfacial reaction. Particularly, carbon nanotubes and certain active metals are easy to generate chemical reaction to generate metal carbide in the high-energy ball milling or sintering process. Tantalum is a strong carbide forming element and is easy to generate TaC with carbon at high temperature. If not controlled, the nano carbon reinforcing phase may be carbonized completely during the sintering process of the target material, and the original shape and function are lost. Therefore, the prior art lacks an effective means in this respect, and no report has been made on successful introduction of the nanocarbon material into the Ta-W target and ensuring that it is not fully carbonized. At present, a Ta-W target preparation process which is specially oriented to a flexible brain-computer interface electrode is not yet seen. For example, in brain-computer interface applications, film internal stress below 100MPa and withstanding tens of thousands of bends without breaking are required, but existing Ta-W films have difficulty meeting this demanding criteria. In addition, the disclosed and reported Ta-W preparation method lacks application of a second phase toughening and magnetic field induced texture process, does not introduce a conductive phase such as nano carbon into the preparation of a Ta-W target, and solves the problems of stress and reliability in flexible electrons by controlling crystal orientation through a magnetic field. Based on the technical blank, an innovative Ta-W based nano composite target preparation method is needed to solve the problems of high internal stress, insufficient bending reliability and the like of a sputtering film when the traditional Ta-W target is applied to a flexible brain-computer interface electrode. Disclosure of Invention In order to solve the technical problems, the invention provides a tantalum-tungsten-based nano composite target and a preparation method thereof. The invention can prepare the Ta-W based nano composite target material with high density, uniform tissue and texture orientation, and the deposited film has the characteristics of low stress, high flexibility and the like, thereby meeting the use requirement of the flexible implantation electrode. In a first aspect, the present in