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Preparation method of molybdenum tube

A technology of molybdenum tube and molybdenum powder, which is applied in the field of refractory metal tube preparation, can solve the problems of difficult production, low density of molybdenum tube billet, uneven grain structure and density of molybdenum tube target, and achieve easy processing and good Deformability, easy welding effect

Inactive Publication Date: 2019-07-12
ZHUZHOU HARD ALLOY GRP CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

On the one hand, the target is required to have a finer and more uniform grain structure, and the average grain size is required to be ≤40 microns. The average grain size of the molybdenum tube target prepared by the existing technology is ≤100 microns, which is difficult to fully meet the use requirements; on the other hand , the size of the molybdenum tube is required to be longer and longer. For example, the length of the molybdenum tube target for the G11 generation TFT-LCD display has exceeded 4 meters. The current cold isostatic pressing + extrusion, cold isostatic pressing + forging, cold isostatic pressing +Hot isostatic pressing technology has been difficult to produce
If the cold isostatic pressing + extrusion process is adopted, the density of the molybdenum tube billet prepared by cold isostatic pressing is low. To achieve high densification, more than 70% of the extrusion deformation is required, and the tonnage of the extrusion equipment is very high. ; The molybdenum tube target grain structure and density produced by the cold isostatic pressing + forging process are not uniform, and it is difficult to meet the sputtering coating requirements of the flat panel display industry; if the cold isostatic pressing + hot isostatic pressing process is used to directly produce more than 4 For a molybdenum tube target with a length of 5 meters, the required cold isostatic pressing and hot isostatic pressing equipment exceeds 5 meters, and the current equipment conditions are difficult to meet the requirements

Method used

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  • Preparation method of molybdenum tube
  • Preparation method of molybdenum tube
  • Preparation method of molybdenum tube

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0041] Select 124Kg of molybdenum powder with a Fibonacci particle size of 2.8 μm; put the molybdenum powder into a stainless steel sheath, and fully vibrate it on a vibrating platform; heat the vibrated stainless steel sheath to 750°C, and evacuate until the vacuum degree is higher than 1 ×10 -2 Pa, keep warm for 2 hours, cool with the furnace, and use argon arc welding for sealing welding; place the sealed stainless steel sheath in a hot isostatic pressing furnace, and the supporting mandrel is a molybdenum alloy rod. Hot isostatic pressing under the condition of 160MPa for 2 hours, and cooled with the furnace, prepared a molybdenum tube blank with an inner diameter of 130mm, an outer diameter of 185mm, and a length of 900mm, and its density was tested to be 10.12g / cm 3 ; Place the molybdenum tube blank in an intermediate frequency induction furnace, heat it at 1250°C for 30 minutes, and then take it out of the furnace for hot extrusion. The extrusion ratio is 2, and the ext...

Embodiment 2

[0043] Select 331Kg of molybdenum powder with a Fibonacci particle size of 3.2μm; put the molybdenum powder into a stainless steel sheath, and fully vibrate it on a vibration platform; heat the vibrated stainless steel sheath to 850°C, and evacuate until the vacuum degree is higher than 5 ×10 -3 Pa, keep warm for 1.5 hours, cool with the furnace, and seal welding with argon arc welding; place the stainless steel sheath for sealing welding in a hot isostatic pressing furnace, and the supporting mandrel is a tungsten alloy rod. Hot isostatic pressing for 3 hours under the condition of 180MPa, and cooled with the furnace to prepare a molybdenum tube billet with an inner diameter of 135mm, an outer diameter of 227mm, and a length of 1250mm. The density was 10.13g / cm after testing. 3 ; Place the molybdenum tube blank in an intermediate frequency induction furnace, heat it at 1300°C for 50 minutes, and then take it out of the furnace for hot extrusion. The extrusion ratio is 2.4. Th...

Embodiment 3

[0045] Select 493Kg of molybdenum powder with a Fibonacci particle size of 3.0 μm; put the molybdenum powder into a stainless steel sheath, and fully vibrate it on a vibration platform; heat the vibrated stainless steel sheath to 800°C, and evacuate until the vacuum degree is higher than 5 ×10 -3 Pa, keep warm for 2.5 hours, then cool with the furnace, and use argon arc welding for sealing welding; place the sealed stainless steel sheath in a hot isostatic pressing furnace, and the supporting mandrel is a tungsten alloy rod. Hot isostatic pressing for 3 hours under the condition of 200MPa, and cooled with the furnace to prepare a molybdenum tube billet with an inner diameter of 135mm, an outer diameter of 244mm, and a length of 1500mm, and its density was tested to be 10.13g / cm 3 ; Place the molybdenum tube blank in an intermediate frequency induction furnace, heat it at 1350°C for 60 minutes, and then take it out of the furnace for hot extrusion. The extrusion ratio is 3, and...

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Abstract

The invention discloses a preparation method of a molybdenum tube for a rotating target material. The method comprises the following steps: 1, carrying out filling and hot isostatic pressing treatmenton molybdenum powder to obtain a molybdenum tube blank; and 2, extruding and annealing the molybdenum tube blank to obtain the molybdenum tube. The method has the advantages of few process steps, short production period and the like; and the molybdenum tube prepared by the method has high density and fine and uniform crystal grain structure, specifically, the density is greater than or equal to 99% of theoretical density, the average crystal grain size is smaller than or equal to 40 [mu]m, the maximum length can exceed 4 meters, and the molybdenum tube can well meet the sputtering coating requirements in the industries of plane display, solar photovoltaic and the like.

Description

technical field [0001] The invention relates to a method for preparing a molybdenum tube, in particular to a method for preparing a molybdenum tube for a rotating target, and the molybdenum tube prepared by the method, belonging to the technical field of refractory metal tube preparation. Background technique [0002] The refractory metal molybdenum has the advantages of high melting point, high strength, low thermal expansion coefficient, low resistivity, good thermal stability, etc. It is widely used in magnetron sputtering coating industries such as flat panel display and solar photovoltaic. Molybdenum sputtering targets can be divided into planar targets and tubular targets in terms of shape. Designs with tubular target structures show substantial advantages over planar targets. Target lifetime is defined as the sputtering power multiplied by the sputtering time (kW·h), or the total thickness of material that can be deposited on the substrate. The change in geometry an...

Claims

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Application Information

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IPC IPC(8): B22F5/12B22F3/15B22F3/20C23C14/34
CPCB22F3/15B22F3/20B22F5/106B22F2003/208B22F2998/10C23C14/3414B22F2003/248
Inventor 魏修宇吴建国刘伟宋立强傅崇伟张外平
Owner ZHUZHOU HARD ALLOY GRP CO LTD
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