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CN-121087440-B - Mo-Ti-Ta-Ce alloy target material and preparation method and application thereof

CN121087440BCN 121087440 BCN121087440 BCN 121087440BCN-121087440-B

Abstract

The invention discloses a Mo-Ti-Ta-Ce alloy target and a preparation method and application thereof, belonging to the technical field of alloy sputtering targets and powder metallurgy. The preparation method of the alloy target comprises the steps of weighing titanium, tantalum, cerium and molybdenum according to atomic percentages of elements, under the protection of inert gas, weighing tantalum powder, cerium dioxide powder and molybdenum powder, performing first ball milling treatment to obtain Mo-Ta-CeO 2 prealloy powder, weighing TiH 2 powder and the rest Mo powder, performing second ball milling treatment to obtain Mo-Ti prealloy powder, uniformly mixing the two prealloy powders, performing cold isostatic pressing to obtain a cold-pressed blank, sintering the cold-pressed blank to obtain a sintered blank, rolling the sintered blank to obtain a rolled target, and annealing the rolled target to obtain the Mo-Ti-Ta-Ce alloy target. The film prepared by the alloy target material has excellent corrosion resistance, oxidation resistance and conductivity.

Inventors

  • HU BOLIANG
  • LI JIA
  • HU PING
  • YE WENTING
  • WANG KUAISHE
  • YANG KE

Assignees

  • 西安建筑科技大学

Dates

Publication Date
20260508
Application Date
20250903

Claims (10)

  1. 1. The preparation method of the Mo-Ti-Ta-Ce alloy target is characterized by comprising the following steps of: Weighing 20-40% of Ti, 5-12% of Ta and 0.05-0.12% of Ce according to the atomic percentage of each element of the Mo-Ti-Ta-Ce alloy target material, wherein the balance of Mo and unavoidable impurities, and the sum of the Mo is more than or equal to 45% and is 100%; Under the protection of inert gas, weighing Ta powder, ceO 2 powder and Mo powder according to 5% -12% of Ta, 0.05% -0.12% of Ce and 15% -21% of Mo, uniformly mixing to obtain first mixed powder, and performing first ball milling treatment on the first mixed powder to obtain Mo-Ta-CeO 2 prealloy powder, wherein in the first ball milling treatment, the ball material ratio is 5-10:1; Under the protection of inert gas, weighing TiH 2 powder according to 20% -40% of Ti, uniformly mixing the TiH 2 powder with the rest of Mo powder to obtain second mixed powder, and performing second ball milling treatment on the second mixed powder to obtain Mo-Ti prealloyed powder, wherein in the second ball milling treatment, the ball-to-material ratio is 2-6:1; mixing Mo-Ta-CeO 2 prealloy powder and Mo-Ti prealloy powder in batches under the protection of inert gas, and carrying out cold isostatic pressing after uniformly mixing to obtain a cold-pressed blank; Sintering the cold-pressed blank in a reducing atmosphere to obtain a sintered blank; And carrying out annealing treatment on the rolled target at 900-1050 ℃ in a reducing atmosphere to obtain the Mo-Ti-Ta-Ce alloy target.
  2. 2. The method for preparing the Mo-Ti-Ta-Ce alloy target according to claim 1, wherein in the first ball milling treatment, the ball milling time is 1.5-3 hours.
  3. 3. The method for preparing the Mo-Ti-Ta-Ce alloy target according to claim 1, wherein in the second ball milling treatment, the ball milling time is 2-4 hours.
  4. 4. The method for preparing the Mo-Ti-Ta-Ce alloy target according to claim 1, wherein when the Mo-Ta-CeO 2 prealloy powder and the Mo-Ti prealloy powder are mixed, a three-dimensional mixer is used, and the mixing time is 4-5 hours.
  5. 5. The method for preparing the Mo-Ti-Ta-Ce alloy target according to claim 1, wherein in the cold isostatic pressing treatment, the pressure is 150-250 MPa, and the dwell time is 6-20 min.
  6. 6. The method for preparing the Mo-Ti-Ta-Ce alloy target according to claim 1, wherein in the sintering treatment, the first-stage heating rate is set to 10 ℃ per minute, the temperature is raised to 950 ℃ to 1100 ℃ and kept for 3.5 to 5 hours, the second-stage heating rate is set to 10 ℃ per minute, the temperature is raised to 1290 ℃ to 1310 ℃ and kept for 1 to 2 hours, and the third-stage heating rate is set to 5 ℃ to 8 ℃ per minute, and the temperature is raised to 1350 ℃ to 1450 ℃ and kept for 4 to 6 hours.
  7. 7. The preparation method of the Mo-Ti-Ta-Ce alloy target material is characterized in that in the rolling treatment, the initial rolling temperature is 1150-1400 ℃, the final rolling temperature is 1000-1200 ℃, the total rolling deformation in the rolling process is controlled to be 45%, the single-pass rolling deformation is controlled to be 15-25%, the heat preservation is carried out at 1050-1100 ℃ before each pass of the hot rolling process, and the heat preservation time is 0.5-1 h.
  8. 8. The method for preparing the Mo-Ti-Ta-Ce alloy target according to claim 1, wherein the annealing time is 1-2 h.
  9. 9. A Mo-Ti-Ta-Ce alloy target material prepared by the preparation method according to any one of claims 1 to 8.
  10. 10. Use of a Mo-Ti-Ta-Ce alloy target according to claim 9 in a magnetron sputtering process for the preparation of thin films.

Description

Mo-Ti-Ta-Ce alloy target material and preparation method and application thereof Technical Field The invention relates to the technical field of alloy sputtering targets and powder metallurgy, in particular to a Mo-Ti-Ta-Ce alloy target and a preparation method and application thereof. Background With the update iteration of flat panel displays such as a Liquid crystal display (Liquid CRYSTAL DISPLAY, LCD), a thin film transistor Liquid crystal display (Thin film transistor Liquid CRYSTAL DISPLAY, TFT-LCD), a plasma display (PLASMA DISPLAY PANEL, PDP), the size specifications of the flat panel displays are more enlarged and the application scenes are more diversified. The continuous progress of the intelligent interconnection technology increases the demand of flat panel displays in different scenes, displays used in various fields such as industry are also faced with more complex service conditions, and the performance requirements on sputtering targets and barrier films in the displays are more strict. The wiring material in flat panel displays or other semiconductor devices is usually low-resistance Al or Cu, but the heating process is involved in the preparation process of the wiring layer of the electronic device, and the direct contact of the Al or Cu conductive layer and the Si semiconductor film at a higher temperature can cause a great deal of diffusion of Al or Cu in Si, so that a molybdenum alloy film needs to be covered between the Al or Cu conductive layer and the Si semiconductor film to serve as a barrier layer. At present, a film sputtered by an alloy target material of a MoTi/MoNiTi system and the like is mainly used as a barrier layer, but the barrier layer film sputtered and deposited by the target material of the component system has the problems of insufficient corrosion resistance, oxidation resistance and high-temperature performance. For example, for flat panel displays used in industrial environments where humidity or acid/alkali and temperature are high, the inner barrier layer is extremely susceptible to moisture, acid-base atmosphere or temperature, and in addition, when the flat panel display is subjected to signal cable wiring operation, the inner structure is exposed to high temperature and oxygen-rich environment for a long time, which requires that the film as the barrier layer has higher corrosion resistance and oxidation resistance. Meanwhile, the corrosion resistance and oxidation resistance of the barrier layer film should be improved on the basis of not damaging or even improving the conductivity of the barrier layer film. Disclosure of Invention Aiming at the problems, the invention provides a Mo-Ti-Ta-Ce alloy target material, a preparation method and application thereof, and when the Mo-Ti-Ta-Ce alloy target material is used for preparing a film, the prepared film has excellent corrosion resistance, oxidation resistance and electrical conductivity. The first object of the invention is to provide a preparation method of a Mo-Ti-Ta-Ce alloy target, which comprises the following steps: According to the atomic percentage of each element of the Mo-Ti-Ta-Ce alloy target, weighing 20% -40% of Ti, 5% -12% of Ta and 0.05% -0.12% of Ce, and the balance being Mo and unavoidable impurities, wherein the sum of the Mo and the unavoidable impurities is more than or equal to 45%, and the total is 100%. Under the protection of inert gas, weighing Ta powder, ceO 2 powder and Mo powder according to 5% -10% of Ta, 0.05% -0.12% of Ce and 15% -21% of Mo, uniformly mixing to obtain first mixed powder, and performing first ball milling treatment on the first mixed powder to obtain Mo-Ta-CeO 2 prealloy powder. Under the protection of inert gas, weighing TiH 2 powder according to 20% -40% of Ti, uniformly mixing the TiH 2 powder with the rest Mo powder to obtain second mixed powder, and carrying out second ball milling treatment on the second mixed powder to obtain Mo-Ti prealloy powder. And mixing the Mo-Ta-CeO 2 prealloyed powder and the Mo-Ti prealloyed powder in batches, and carrying out cold isostatic pressing after uniformly mixing to obtain a cold-pressed blank. And sintering the cold-pressed blank in a reducing atmosphere to obtain a sintered blank. And carrying out annealing treatment on the rolled target at 900-1050 ℃ in a reducing atmosphere to obtain the Mo-Ti-Ta-Ce alloy target. In a preferred embodiment of the invention, in the first ball milling treatment, the ball-to-material ratio is 5-10:1, and the ball milling time is 1.5-3 hours. In a preferred embodiment of the invention, in the second ball milling treatment, the ball-to-material ratio is 2-6:1, and the ball milling time is 2-4 hours. In a preferred embodiment of the invention, when the Mo-Ta-CeO 2 prealloyed powder and the Mo-Ti prealloyed powder are mixed, a three-dimensional mixer is used, and the mixing time is 4-5 hours. In a preferred embodiment of the invention, the pressure in the cold isostatic pressing treatment