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A kind of preparation method of long molybdenum tube sputtering target

A technology for sputtering target material and molybdenum tube, which is applied in the field of preparation of long molybdenum tube sputtering target material, can solve the problems that the forging method is difficult to meet the density requirements, it is difficult to control the thermal deformation of the molybdenum tube, and the raw material particle size requirements are very high. Conducive to splicing, small gap and low oxygen content

Active Publication Date: 2019-09-03
OMAT ADVANCED MATERIALS (GUANGDONG) CO LTD +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] At present, the method of preparing large-size molybdenum tube target is mainly sintering method, but this method has high requirements on the particle size of raw materials, and the sintering density is low, it is difficult to meet the density requirement of 99.5%. In addition, long molybdenum tubes are easy to bend and deform during the sintering process. Low yield
In addition to the sintering method, there are three preparation methods: hot pressing, extrusion and forging. However, the hot pressing method easily leads to excessive impurities and oxygen content, and cannot meet the purity requirement greater than 99.95%. The pressing equipment must be able to withstand a pressure greater than 5,000 tons, which requires high equipment; the forging method is difficult to meet the 99.5% density requirement, and at the same time, it is difficult to control the thermal deformation of the molybdenum tube during the forging process, which also leads to poor internal uniformity of the molybdenum tube

Method used

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  • A kind of preparation method of long molybdenum tube sputtering target
  • A kind of preparation method of long molybdenum tube sputtering target
  • A kind of preparation method of long molybdenum tube sputtering target

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preparation example Construction

[0034] The preparation method of long molybdenum tube sputtering target material of the present invention comprises the following steps:

[0035] S1 Molybdenum tube billet pressing: Weigh molybdenum powder with a purity of ≥99.99% and put it into the mixer, vacuumize it and fill it with argon, then stir and mix it in an argon environment for 5-8 hours to obtain a mixed molybdenum powder, and mix it Evenly put the molybdenum powder into the tubular cavity of the cold isostatic pressing mold, press the molybdenum powder into a tubular shape under the cold isostatic pressing of 150-200MPa, and then remove the cold isostatic pressing mold to obtain the molybdenum tube billet, and the end of the molybdenum tube billet The head and the outer surface are trimmed to make it smooth;

[0036] S2 sintered molybdenum tube blank: place the trimmed molybdenum tube blank in a hydrogen environment and sinter at 1800-2000°C for 4-10h, and trim the ends and inner and outer surfaces of the sinte...

Embodiment 1

[0045] S1 pressed molybdenum tube billet

[0046] Put molybdenum powder with a purity ≥ 99.99%, an average Fischer particle size of 2-6 μm, and an oxygen content of <500 ppm into a V-type mixer, vacuumize and fill with argon, then fully stir and mix in argon for 5 hours to obtain Mixed molybdenum powder;

[0047] Evenly mix the molybdenum powder into the cold isostatic pressing cylinder mold through the vibrating platform. After the molybdenum powder fills the tubular cavity, tamp it evenly and tighten the end of the rubber sleeve. Under the cold isostatic pressing pressure of 150Pa Press the molybdenum powder into a tube, then remove the mandrel from the mold to obtain a molybdenum tube blank with a theoretical density of 60%-65% and a length of 520-530mm, and then machine and trim the two ends and the outer surface of the molybdenum tube blank to ensure that the outer surface Uniform without dents or bumps.

[0048] S2 sintered molybdenum tube billet

[0049] Sinter the t...

Embodiment 2

[0055] S1 pressed molybdenum tube billet

[0056] Put molybdenum powder with a purity ≥ 99.99%, an average Fischer particle size of 2-6 μm, and an oxygen content of <500 ppm into a V-shaped blender, vacuumize and fill with argon, then fully stir and mix in argon for 8 hours to obtain Mixed molybdenum powder;

[0057] Put the evenly mixed molybdenum powder into the cold isostatic pressing cylinder mold through the vibration platform. After the molybdenum powder fills the tubular cavity, tamp it evenly and tighten the end of the rubber sleeve. Under the cold isostatic pressure of 200MPa Press the molybdenum powder into a tube, then remove the mandrel from the mold to obtain a molybdenum tube blank with a theoretical density of 60%-65% and a length of 700-710mm, and then machine and trim the two ends and the outer surface of the molybdenum tube blank to ensure that the outer surface Uniform without dents or bumps.

[0058] S2 sintered molybdenum tube billet

[0059] Sinter the...

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Abstract

The invention relates to a preparation method of a long molybdenum tube sputtering target material. The method comprises the following steps that S1, molybdenum tube blanks are pressed; specifically,evenly-mixed molybdenum powder is put into a tubular cavity of a cold isostatic pressing die, the molybdenum powder is pressed into tubes at 150-200 MPa, then the cold isostatic pressing die is disassembled, the molybdenum tube blanks are obtained, and the ends and outer circles of the molybdenum tube blanks are trimmed; S2, the molybdenum tube blanks are sintered, specifically, the molybdenum tube blanks are arranged in a hydrogen atmosphere to be sintered at 1800-2000 DEG C for 4-10 hours, and the sintered molybdenum tube blanks are trimmed; S3, the long molybdenum tube is spliced, specifically, the multiple molybdenum tube blanks obtained in the S2 are longitudinally and sequentially stacked in a tubular cavity of a hot isostatic pressing die, then the airtightness of the tubular cavityis inspected, the molybdenum tube blanks qualified in airtightness are selected for hot isostatic pressing treatment, and the long molybdenum tube is obtained and wrapped with the hot isostatic pressing die; and S4, the long molybdenum tube is straightened, specifically, the hot isostatic pressing die wrapping the long molybdenum tube is subjected to heat straightening treatment, the die is disassembled, and the long molybdenum tube sputtering target material is obtained.

Description

technical field [0001] The invention relates to the technical field of target production, in particular to a method for preparing a long molybdenum tube sputtering target. Background technique [0002] Molybdenum targets are widely used in conductive glass, STN / TN / TFT-LCD, optical glass, ion coating and other industries, and are suitable for all flat coating and rotary coating systems. [0003] At present, the method of preparing large-size molybdenum tube target is mainly sintering method, but this method has high requirements on the particle size of raw materials, and the sintering density is low, it is difficult to meet the density requirement of 99.5%. In addition, long molybdenum tubes are easy to bend and deform during the sintering process. The yield is low. In addition to the sintering method, there are three preparation methods: hot pressing, extrusion and forging. However, the hot pressing method easily leads to excessive impurities and oxygen content, and cannot ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B22F9/04B22F3/04B22F3/10B22F3/15B22F3/24B22F5/12C22C27/04
CPCB22F3/04B22F3/1007B22F3/15B22F3/24B22F5/106B22F9/04B22F2003/248B22F2009/041B22F2998/10B22F2999/00C22C27/04B22F2201/11B22F2201/013B22F2201/20
Inventor 李培林文宏福
Owner OMAT ADVANCED MATERIALS (GUANGDONG) CO LTD