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Ru sputtering target with high purity and preparation method thereof

A sputtering target and high-purity technology, applied in the field of powder metallurgy, can solve the problems of unusable molds, increase production costs, large losses, etc., and achieve the effects of reducing abnormal discharge phenomena, saving production costs, and improving production efficiency

Inactive Publication Date: 2012-07-25
KUNMING INST OF PRECIOUS METALS
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although this method prepares a high-purity Ru target with low C and O content, the coating used and the pressed ruthenium block have a thicker diffusion layer, which leads to greater loss during subsequent processing, and the mold dies after each hot pressing and sintering. It cannot be used continuously and needs to be replaced frequently, which greatly increases the production cost and is not conducive to industrial production
At the same time, due to the use of unidirectional pressure for pressing, when the number of pressed blocks increases, the density of the lower target material is lower. In addition, the patent does not disclose the grain size and structure uniformity of the Ru target.

Method used

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  • Ru sputtering target with high purity and preparation method thereof
  • Ru sputtering target with high purity and preparation method thereof
  • Ru sputtering target with high purity and preparation method thereof

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preparation example Construction

[0032] The present invention has prepared the above-mentioned high-purity ruthenium sputtering target material through the following method. The ruthenium sputtering target is prepared by a two-way vacuum hot pressing method. The specific preparation method includes the following steps:

[0033] (1) Powder pretreatment: the high-purity ruthenium powder is ball milled and graded, and the particle size of the ruthenium powder for the sintered target is 1-10 μm;

[0034] (2) powder filling: the ruthenium powder is filled in the graphite mold through the powder loading device;

[0035] (3) Powder sintering: send the mold containing high-purity ruthenium powder into a vacuum hot-pressing sintering furnace for two-way vacuum hot-pressing sintering with a vacuum degree of 10 -2 ~10 -4 pa, the sintering temperature is 1100-1800°C, the sintering pressure is 30-60MPa, and the holding time is 1-5h.

[0036] The ball mill crushing technique of described high-purity ruthenium powder is t...

Embodiment 1

[0042] The high-purity ruthenium sputtering target of the present invention is made through the following steps:

[0043](1) Powder pretreatment: select high-purity Ru powder with a purity of 3N5, and carry out planetary ball milling to the high-purity Ru powder. The grinding medium is yttrium-stabilized zirconia balls with a diameter of 2 mm and a ball-to-material ratio of 3: 1 (mass ratio), the revolution speed of the ball mill is 500rpm, and the ball milling time is 5min. After the ball milling, the ruthenium powder with a particle size of 1-10 μm is obtained and used as raw material powder.

[0044] (2) Powder filling: put the raw material powder required for 5 targets into the graphite mold through the powder filling device (such as figure 1 shown), the middle is separated by a graphite gasket, and 5 targets are pressed and formed at the same time.

[0045] (3) Powder sintering process: Put the graphite mold filled with Ru powder into the furnace body of vacuum two-way h...

Embodiment 2

[0047] The difference from Example 1 is that the ball mill crushing process is as follows: the diameter of the yttrium stabilized zirconia ball is 6 mm, the ball-to-material ratio is 6:1, the ball mill speed is 400 rpm, and the ball mill crushing time is 30 min. The sintering process is as follows: the sintering temperature is 1800°C, the sintering pressure is 30MPa, and the sintering vacuum is 10 -2 ~10 -3 Pa, from room temperature to 600°C, the heating rate is 15°C / min, keep at 600°C for 30 minutes, then continue to increase the temperature, the heating rate is 10°C / min, when the temperature rises to 1300°C, keep the temperature for 1 hour, and then continue Raise the temperature at a rate of 5°C / min. When the temperature rises to 1800°C, keep it at this temperature for 1 hour.

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Abstract

The invention discloses an Ru sputtering target with a high purity and a preparation method of the target. The density of the Ru sputtering target is higher than 99%, and the average crystal grain size is 2-10 microns. The specific preparation method comprises the following steps: (1) pretreating powder; (2) filling the powder; and (3) sintering the powder: sending a mold filled with the high-purity Ru powder into a vacuum hot-pressing sintering furnace and performing bidirectional vacuum hot pressing and sintering, wherein the vacuum degree is 10<-2>Pa to 10<-4>Pa, the sintering temperature is 1100-1800 DEG C, and the sintering pressure is 30-60MPa. According to the invention, the Ru sputtering target is prepared by the bidirectional vacuum hot-pressing and sintering technology, the density is higher than 99%, the average crystal grain size is 2-10 microns, and the boundary and the core microstructure are uniform. The target used for magnetron sputtering can reduce paradoxical discharge in the sputtering process and can improve the sputtering speed rate and the uniformity of distribution of the film thickness. Meanwhile, by adopting the bidirectional pressing method, multiple pieces in one furnace can be synchronously pressed, and the related performance such as structural uniformity of the pressed target is equal to the performance of hot isostatic pressing, so that the production efficiency is improved, the production cost is saved and the power consumption is reduced.

Description

technical field [0001] The invention belongs to the technical field of powder metallurgy, and in particular relates to a high-purity Ru sputtering target and a preparation method thereof. Background technique [0002] Ru and Ru-based alloy materials are widely used in the manufacture of many electronic products, such as the intermediate transition layer in high-density perpendicular magnetic recording media, the coupling layer in high-performance, high-area recording density antiferromagnetic coupling magnetic recording media And as an adhesion layer / seed layer in copper-based back-end metallization systems for high-integration-density semiconductor integrated circuit devices. These thin film layers are generally formed using Ru or Ru-based alloy targets as raw materials by sputtering deposition techniques such as magnetron sputtering. Generally speaking, these applications require that the sputtering target used has less impurity content, uniform structure composition, hig...

Claims

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Application Information

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IPC IPC(8): C23C14/34C23C14/35C23C14/14B22F3/14
Inventor 谭志龙管伟明张昆华杨杰毕珺王传军陈松张俊敏李艳琼
Owner KUNMING INST OF PRECIOUS METALS
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