Tungsten alloy target material and preparation method thereof

A technology of tungsten alloy and target material, which is applied in the field of high-density tungsten alloy target material and its preparation, can solve the problems of unfavorable discharge intermittent sintering of particle pores, unfavorable sintering of large-size products, uneven temperature distribution, etc., to increase density and sintering time, reducing sintering time, and inhibiting the effect of grain growth

Active Publication Date: 2013-01-23
FOSHAN JUSHITAI POWDER METALLURGY CO LTD
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  • Abstract
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  • Application Information

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Problems solved by technology

[0015] It can be seen from the existing literature and reports that in the current W / Ti alloy sintering, generally include hot pressing (vacuum hot pressing and inert gas hot pressing), hot isostatic pressing, thermal explosion synthesis and recent The spark plasma sintering method, and the compactness of the targets of the first three methods is relatively good, but they are often limited by the requirements of the target on size, micro-morphology and low cost. At the same time, the sintering time is longer, from From the perspective of energy, its economic benefit is not high; the pressure requirement is high, the wear and tear on the mold is great, and its equipment cost is high
A spark plasma sintering technology that has emerged in recent years has the characteristics of rapid sintering of dense materials at lower temperatures, but it puts forward higher requirements for its powder to be fully sintered and dense. Uneven distribution, and when a certain density is reached, the particle pores become smaller, which is not conducive to intermittent discharge sintering, especially not conducive to the sintering of large-sized products, resulting in inconsistent density between the center and the periphery
The above-mentioned DC sintering, the thermal effect generated by the current, can be adapted to large-scale sintering, but the long time will lead to uneven phase composition and grain growth
Up to now, there has not been a method for preparing W / Ti alloy targets with high efficiency, fine and uniform microstructure, high density, large size, low cost preparation, and relatively short sintering time.

Method used

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  • Tungsten alloy target material and preparation method thereof

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Experimental program
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Effect test

Embodiment 1

[0043] Sintering mode: variable voltage, fixed pulse current and fixed direct current dual-mode sintering, using devices such as figure 1 As shown, the operation steps are as follows figure 2 shown.

[0044] W powder with an average particle size of 0.5-30 μm (purity 99.99%), Ti powder with an average particle size of 20-30 μm (purity 99.99%) and yttrium powder with an average particle size of 20-30 μm (purity 99.99%), according to Weigh at a weight ratio of 89.8:10:0.2, ball mill for 4 hours under the protection of inert gas (Ar gas) and mix evenly, then place it in a rectangular high-strength, high-temperature-resistant and insulating mold of 800mm×580mm. Sintering with fixed pulse current and fixed direct current dual mode. Pre-compact and evacuate to 5×10 -4 Pa, start direct current direct heating sintering, the direct current density is 2.80mA / mm 2 , heat up to 1200°C, hold for 8 minutes, during which the pressure is continuously increased from 10MPa to 30MPa; mainta...

Embodiment 2

[0046] Sintering mode: variable voltage type, variable frequency variable amplitude pulse current and fixed direct current dual mode sintering, using devices such as figure 1 As shown, the operation steps are as follows figure 2 shown.

[0047] W powder (purity 99.99%) with an average particle size of 0.5-30 μm and Ti powder (purity 99.99%) with an average particle size of about 30 μm were weighed in a ratio of 80:20 by weight, in an inert gas (Ar gas) After ball milling under protection for 5 hours to mix evenly, place it in an 800mm×580mm rectangular high-strength, high-temperature-resistant and insulating mold. Sintering with variable frequency and variable amplitude pulse current and fixed direct current dual mode. Pre-compacted and evacuated to 3.2 x 10 -4 Pa, ion sintering at a temperature of 1400°C, where the pulse current density ranges from 11.67mA / mm 2 increased to 14.58mA / mm 2 , and the frequency is reduced from 82Hz to 65Hz, the duty cycle is constant at 89%,...

Embodiment 3

[0049] Sintering mode: variable voltage type, fixed pulse current and variable direct current dual mode sintering, using devices such as figure 1 As shown, the operation steps are as follows figure 2 shown.

[0050] W powder (purity 99.99%) with an average particle size of 0.5-30 μm, TiH with an average particle size of 10-30 μm 2 powder (purity 99.99%), weighed in a ratio of 90:10 by weight, ball milled for 7 hours under the protection of an inert gas (Ar gas) and mixed evenly, then placed in a rectangular high-strength, high-temperature-resistant and insulating mold of 800mm × 580mm Inside. Using fixed pulse current and variable direct current dual mode sintering, pre-compacted and vacuumed to 2.5×10 -4 Pa, turn on the DC and pulse current source, when the DC voltage is fixed at 400V, the current density changes from 2.81mA / mm over time 2 Slowly change to 3.31mA / mm 2 , at the same time, the pulse current frequency is 80Hz, and the density is 12.71mA / mm 2 , the duty cy...

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Abstract

The invention discloses a high-temperature tungsten alloy target material with large size, high density and high purity and a preparation method thereof. In the preparation method, a unique voltage transformation and dual-mode combination sintering technology is adopted. The method comprises the following step of: sintering raw material powder of the target material in a plasma discharge and direct current dual-mode combination mode under vacuum and voltage transformation to obtain the tungsten alloy target material. By the technology, the large-size refractory alloy target material of which the density is more than 99.98 percent TD and the ingredients and microstructures are uniform and controllable can be prepared, and the aims of high performance and large size which cannot be realizedin the conventional preparation technology of the high-temperature refractory alloy target material are fulfilled. Simultaneously, the high-temperature tungsten alloy target material has the characteristics of short sintering time, high energy efficiency and small loss of equipment and dies, and production cost and preparation cost are reduced effectively.

Description

technical field [0001] The invention belongs to the technical field of preparation of refractory alloy targets, in particular to a high-density tungsten alloy target and a preparation method thereof. Background technique [0002] The sputtering coating method is the main method in the coating technology. It has the outstanding advantages of high coating efficiency, a wide range of applicable materials, and controllable film thickness, composition, structure and performance. It is widely used in various metals, semiconductors, ceramics and other functional and The preparation of structural thin film materials, as well as the surface treatment of various components and the preparation of devices. The composition ratio, microstructure and uniformity, purity, density, and target size of the target have a very important impact on the composition, structure, performance and coating efficiency of the final film. With strict composition ratio, delicate structure, high purity (>9...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B22F3/105C23C14/34
Inventor 崔明培王家生任山朱湘平
Owner FOSHAN JUSHITAI POWDER METALLURGY CO LTD
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