A method for improving grain uniformity of molybdenum and its alloy sputtering targets

A technology of sputtering target material uniformity, applied in sputtering coating, metal material coating process, vacuum evaporation coating, etc. inequality problem

Active Publication Date: 2020-10-20
ZHENGZHOU UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The local unevenness of the target grains will cause local unevenness of the coating thickness, and as the sputtering process proceeds, the large grains will form a "mountain phenomenon" and finally fall off suddenly, which will affect the quality of the coating and cause the device Poor functional consistency and short service life; the difference in average grain size between different regions of the target will cause the film thickness of the large coated plate to be different between different regions, and the film thickness of the small coated plate obtained by cutting is different, making the electronic Component performance consistency decline

Method used

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  • A method for improving grain uniformity of molybdenum and its alloy sputtering targets
  • A method for improving grain uniformity of molybdenum and its alloy sputtering targets
  • A method for improving grain uniformity of molybdenum and its alloy sputtering targets

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] A method for improving the uniformity of the crystal grains of a molybdenum sputtering target material (the target material is pure molybdenum), which specifically includes the following steps:

[0031] 1) Use industrial molybdenum powder with a Fischer particle size of 2.9μm and mill it in a ball mill for 8 hours, with a ball-to-battery ratio of 2:1. Then classify to obtain molybdenum powder with a Fischer particle size of 3.2 μm, in which the content of particles below 1 μm is 4.5%, and the content of particles below 0.5 μm is 0.8%;

[0032] 2) The molybdenum powder obtained in step 1) is formed by cold isostatic pressing to obtain a pressed slab with a pressing pressure of 1.6 tons / cm 2 , The thickness of the pressed slab is 35mm;

[0033] 3) The pressed slab is sintered in a microwave-resistance vacuum furnace. After the microwave is heated to 1500℃, it is changed to resistance heating, and the heating speed is controlled to make the vacuum degree of the heating process 1×...

Embodiment 2

[0044] A method for improving the uniformity of crystal grains of molybdenum sputtering target material, which specifically includes the following steps:

[0045] 1) Use industrial molybdenum powder with a Fischer particle size of 3.5μm and mill it in a ball mill for 5 hours, with a ball-to-battery ratio of 2:1. Then classify to obtain molybdenum powder with a Fischer particle size of 3.7 μm, in which the content of particles below 1 μm is 3.9%, and the content of particles below 0.5 μm is 0.65%;

[0046] 2) The molybdenum powder obtained in step 1) is formed by cold isostatic pressing to obtain a pressed slab with a pressing pressure of 1.8 tons / cm 2 , The thickness of the pressed slab is 29mm;

[0047] 3) The pressed slab is sintered in a microwave-resistance vacuum furnace. After the microwave is heated to 1500℃, it is changed to resistance heating, and the heating speed is controlled to make the vacuum degree of the heating process 1×10 -2 Below Pa, the vacuum degree of the heat ...

Embodiment 3

[0053] A method for improving the uniformity of crystal grains of molybdenum sputtering target material, which specifically includes the following steps:

[0054] 1) Use industrial molybdenum powder with a Fischer particle size of 4.2μm and mill it in a ball mill for 4 hours, with a ball-to-battery ratio of 2:1. Then classify to obtain molybdenum powder with a Fischer particle size of 4.3 μm, of which 2.4% of particles below 1 μm and 0.3% of particles below 0.5 μm;

[0055] 2) The molybdenum powder obtained in step 1) is formed by cold isostatic pressing to obtain a pressed slab with a pressing pressure of 2 tons / cm 2 , The thickness of the pressed slab is 22mm;

[0056] 3) The pressed slab is sintered in a microwave-resistance vacuum furnace. After the microwave is heated to 1500℃, it is changed to resistance heating, and the heating speed is controlled to make the vacuum degree of the heating process 1×10 -2 Below Pa, the vacuum degree of the heat preservation stage is 1×10 -3 Belo...

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Abstract

The invention relates to a method for improving molybdenum and alloy sputtering target material grain uniformity. The method comprises the steps that firstly, molybdenum powder with the fisher particle size being 2.0 to 4.5 micrometers is subject to ball grinding and grading, and the content of particles, below one micrometers, in the molybdenum powder is below 5%, the content of particles, below0.5 micrometer, in the molybdenum powder is below 1%, and the molybdenum powder is mixed with alloy powder with the fisher particle size being 5 to 20 micrometers evenly to obtain mixed powder; secondly, the mixed powder is subjected to cold isostatic pressing forming, and a pressing plate blank is obtained; thirdly, the pressing plate blank is sintered at the temperature of 1750 to 2150 DEG C andis subjected to heat preservation for 2 to 8 hours, and a sintering blank is obtained; fourthly, the sintered blank is rolled and deforms to obtain a rolled blank, the cogging temperature ranges from1350 to 1500 DEG C, and the final rolling temperature ranges from 1100 to 1400 DEG C; fifthly, the rolled blank is annealed for one to four hours in the vacuum or hydrogen atmosphere at the temperature of 1050 to 1250 DEG C, and the sputtering target material is obtained. Through the method, the grain uniformity in the molybdenum and alloy sputtering target material small area and between the areas can be improved, the sputter coating microcosmic and whole uniformity can be ensured, and the quality, the service life and the product consistency of related electronic element function films canbe improved.

Description

Technical field [0001] The invention belongs to the technical field of preparation and processing of rare metal materials, and in particular relates to a method for improving the uniformity of crystal grains of molybdenum and alloy target materials for sputtering coating. Background technique [0002] Sputtering is the use of ions generated by an ion source to accelerate the accumulation of high-speed ion currents in a vacuum to bombard the solid surface, so that the atoms on the solid surface leave the target and deposit on the surface of the substrate, thereby forming a nanometer (or micrometer) film. The bombarded solids are called sputtering targets. Sputtering coating is the basic method for preparing functional thin films in the fields of integrated circuits, flat panel displays (including liquid crystal displays and touch screens), thin-film solar cells and LEDs. Sputtering targets have become indispensable basic materials in these fields. [0003] With the continuous impro...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C23C14/34C22F1/18C22F1/02C22C1/04
CPCC22C1/045C22F1/02C22F1/18C23C14/3414
Inventor 李庆奎杨凯军吴小超刘振新卢小凯
Owner ZHENGZHOU UNIV
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