A kind of preparation method of high-purity ruthenium sputtering target material

A sputtering target, high-purity technology, applied in the field of powder metallurgy, can solve problems such as extremely high equipment conditions, heavy power system load, and reduced target purity, and achieve stable sputtering performance, less processing and deformation processes, Simple preparation process

Active Publication Date: 2020-08-28
广州海普电子材料科技有限公司
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  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The process of electron beam smelting is complicated, the smelting process has extremely high requirements on equipment conditions, and the power system load is heavy, so the preparation cost is very high
In addition, ruthenium is a high-temperature refractory metal with a melting point as high as 2310°C. The preparation environment is a high-temperature environment, and impurities in the crucible, heating element, heat preservation parts and other environments can easily enter the melt, resulting in impurities mixed in the preparation of high-purity targets. Product performance is very unfavorable
The subsequent processing of the ingot requires repeated plastic processing and heat treatment, and these processes have buried hidden dangers for the reduction of target purity.

Method used

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  • A kind of preparation method of high-purity ruthenium sputtering target material
  • A kind of preparation method of high-purity ruthenium sputtering target material
  • A kind of preparation method of high-purity ruthenium sputtering target material

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preparation example Construction

[0029] A preparation method for a high-purity ruthenium sputtering target, comprising the steps of:

[0030] Step 1. Crushing: use a crusher to crush the high-purity ruthenium block raw materials with a purity of more than 99.95%, vibrate and sieve to obtain a powder with a particle size of less than 500 μm; the inner lining of the crusher is equipped with pure ruthenium with a purity of more than 99.95% coating;

[0031] Step 2. Ball milling: The crushed powder with a particle size of less than 500 μm is ball milled in a nitrogen atmosphere. The ball milling balls are mixed with 3 kinds of high-purity ruthenium balls with different diameters. The purity of the ball milling balls is above 99.95%, and the ball milling is carried out until the particle size is below 200 μm. After ball milling, multi-stage screening is carried out (using multi-layer screens with different apertures to screen step by step) to obtain various particle size grades (using two adjacent layers of screen...

Embodiment 1

[0041] The industrially purified high-purity ruthenium block with a purity of more than 99.95% is broken into small particles below 500 μm by a crusher, and ball milled under a nitrogen protective atmosphere. The diameters of the ball milling balls are: 5mm, 10mm, and 15mm. The ratio of the number of the ball is 9:4:1, the ratio of the total mass of the ball to the mass of the material is 3:1, the ball milled to a particle size below 200 μm, and the volume average particle size is 60 μm; the X-ray of the high-purity Ru powder before sieving after ball milling Diffraction pattern such as figure 1 As shown, the diffraction peak shows only the pure ruthenium phase, and the powder does not contain other phases, so the cleanliness is very high; from the basic principle of phase analysis, the intensity of the XRD diffraction peak shows the crystallization degree of the material, and the higher the diffraction peak intensity is Higher, indicating that the crystallization is more perf...

Embodiment 2

[0043] The difference from Example 1 is that in the ball milling step, the diameters of the ball milling balls are respectively: 5mm, 8mm, and 13mm, the number ratio of the three kinds of balls is 9:3:2, and the ratio of the total mass of the balls to the material mass is 2: 1. Ball mill until the particle size is less than 200 μm and the volume average particle size is 63 μm; in the mold loading step, take three particle size grades of powders with a particle size of less than 10 μm, 60-80 μm, and 140-160 μm, and the mass ratio is 2:4: The ratio of 1 is mixed evenly; in the unidirectional hot pressing molding step, when the temperature is from room temperature to 1000 °C, the heating rate is 10 °C / min; when the temperature is 1000 to 1500 °C, the heating rate is 7 °C / min, and the temperature is When the temperature reaches 1600°C, the heating rate is 4°C / min; while the temperature is rising, pressurization is started, and the applied pressure is 10MPa; the final temperature is...

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Abstract

The invention relates to the technical field of powder metallurgy, in particular to a preparation method of a high-purity ruthenium sputtering target. The method mainly comprises the steps of crushing, ball milling, die filling, one-way hot press molding and the like. In the die filling process, three kinds of powder with different granularities are adopted for mutual filling, and finally sinter molding is carried out. A powder metallurgy is adopted, the target can be prepared at the temperature lower than the material smelting point, the operation difficulty of equipment is greatly lowered, introduction of impurities is also effectively controlled in the preparation process, controllable preparation of target structure fineness can also be achieved by controlling the raw material high-purity ruthenium powder granularity and the sintering technology system, therefore, the target product quality stability is improved, meanwhile, the production cost is greatly reduced, and the high-performance low-cost high-purity ruthenium target with the uniform and controllable microstructure can be obtained.

Description

technical field [0001] The invention relates to the technical field of powder metallurgy, in particular to a method for preparing a high-purity ruthenium sputtering target. Background technique [0002] As a key technology in the manufacture of integrated circuits and chips, magnetron sputtering coating has many advantages such as simple equipment, easy control, and high film uniformity. Among them, the quality of the sputtering target has a decisive influence on the coating effect of magnetron sputtering and the performance of semiconductor devices. Therefore, high-quality sputtering targets have become an indispensable key material for the electronic information technology industry. The film quality (such as film thickness, uniformity, etc.) formed after target sputtering will significantly affect the performance of electronic products such as integrated circuits and chips, and the film quality depends largely on the organizational characteristics of the sputtering target ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C23C14/35B22F9/04B22F3/14
CPCB22F3/14B22F9/04B22F2003/145B22F2009/043C23C14/3414C23C14/35
Inventor 逯峙游龙郭帅东王广欣韩超张鹏飞杨斌闫焉服孙浩亮李海涛
Owner 广州海普电子材料科技有限公司
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