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Molybdenum-niobium alloy rotating target material and preparation method thereof

A molybdenum-niobium alloy and rotating target technology, which is applied in metal processing equipment, metal material coating technology, ion implantation plating, etc., can solve problems such as difficult to reach high-end customers, unsatisfactory, new impurity element pollution, etc., to improve the composition Uniformity and density, the effect of improving the uniform distribution of grain size, controlling deformation and dimensional accuracy

Active Publication Date: 2019-08-23
广东欧莱高新材料股份有限公司 +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] 1. Sintering method: This method has high requirements on the particle size of raw materials, and can quickly realize densified molding and sintering, but the sintering density is low, about 95%, and it is difficult to meet the density requirement of more than 99%.
At the same time, if the sintering deformation of the long tube target is large, it is difficult to correct it later, and it is impossible to produce large-size tube targets
[0005] 2. Hot pressing method: the raw material molybdenum powder and niobium powder are mixed in proportion and pressed into a green body, the green body is crushed and ground to make a secondary powder (large particle powder), and then the secondary powder is put into a sealed mold for pressing Sintering to make a molybdenum-niobium tube target. This method is very easy to introduce new impurity element pollution in the secondary pulverization process, and it is difficult to deoxidize during the sealed pressure sintering process, which will lead to excessive impurities and oxygen content in the product, which cannot meet the existing high-purity molybdenum. Niobium target requirements
[0006] 3. Plasma spraying method: the sputtering layer is prepared by plasma spraying on the surface of stainless steel or other materials, but the prepared sputtering layer has high impurity content, poor compactness, and high cost, which is not suitable for large-scale molybdenum Production of niobium rotating targets
At present, the density of molybdenum-niobium alloy targets produced by most domestic manufacturers is 9.4-9.7g / cm 3 Between, it is difficult to achieve high-end customer density ≥ 9.9g / cm 3 Requirements, especially for products with pipe length requirements within 1000-3000mm, there are holes in the organization, coarse and uneven grains, and the quality is difficult to meet the sputtering target requirements of high-end liquid crystal display and electronics industries.

Method used

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  • Molybdenum-niobium alloy rotating target material and preparation method thereof
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  • Molybdenum-niobium alloy rotating target material and preparation method thereof

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Embodiment 1

[0035] The preparation method of the molybdenum-niobium alloy rotating target described in this embodiment comprises the following steps:

[0036] 1) Preparation of large-particle molybdenum-niobium powder: use high-purity (purity ≥ 99.99%) molybdenum powder and niobium powder raw materials, oxygen content ≤ 500ppm, average Fisherman’s particle size is 4-8 microns, and the ratio of the two powders according to the niobium content is The proportion of 5at% is placed in a V-type mixer, and the argon gas is continuously introduced for 30 minutes after vacuuming, and then fully mixed, and the mixing time is 5-8 hours to obtain a mixed powder; Under the pressure of -1000T, it is pressed into a small billet with a size of 100*100*30mm, and its density is 45-50% of the theoretical value of the density of the molybdenum-niobium alloy; then the billet is refined into a large particle molybdenum-niobium powder by a mechanical crushing ball mill , the ball-to-material ratio during ball m...

Embodiment 2

[0045] The preparation method of the molybdenum-niobium alloy rotating target described in this embodiment comprises the following steps:

[0046] 1) Preparation of large-particle molybdenum-niobium powder: use high-purity (purity ≥ 99.99%) molybdenum powder and niobium powder raw materials, oxygen content ≤ 500ppm, average Fisherman’s particle size is 4-8 microns, and the ratio of the two powders according to the niobium content is The proportion of 15at% is placed in the V-type mixer, and the argon gas is continuously introduced for 30 minutes after vacuuming, and then fully mixed, and the mixing time is 5-8 hours to obtain a mixed powder; Under the pressure of -1000T, it is pressed into a small billet with a size of 100*100*30mm, and its density is 45-50% of the theoretical value of the density of the molybdenum-niobium alloy; then the billet is refined into a large particle molybdenum-niobium powder by a mechanical crushing ball mill , The ball-to-material ratio during bal...

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Abstract

The invention discloses a molybdenum-niobium alloy rotating target and a preparation method thereof. Molybdenum powder and niobium powder are contained into a mold, under the cold isostatic pressure effect, a large-size hollow molybdenum-niobium pipe pressed blank is formed, then containing into a package sheathing for vacuum welding sealing is performed, a pipe blank is formed due to hot isostatic pressure sintering, and after later-period machining, finally a molybdenum-niobium rotating target material is made. According to the preparation method, introduction of impurity elements can be reduced, and the produced target material is uniform is component, free of segregation and tiny in grain. By detecting the obtained molybdenum-niobium alloy rotating target, the density of the rotating target is larger than 9.97g / cm<3>, the grain size is smaller than 50 microns, C-SCAN displays that a structure is uniform, no internal defects are found, and the requirement of a high-end sputtering target material is met.

Description

technical field [0001] The invention relates to the technical field of metal target production, in particular to a molybdenum-niobium alloy rotating target and a preparation method thereof. Background technique [0002] At present, flat panel display (FPD), including liquid crystal display TFT-LCD, plasma display PDP and touch screen TP, etc. have become the mainstream of displays. As the key material of FPD, molybdenum-niobium alloy has been widely used in LCD source matrix liquid crystal display, plasma display bipolar PDP, TFT flexible display, touch screen, OLED and other fields. In recent years, the tubular molybdenum alloy sputtering target with higher utilization rate has been extensively researched and applied by foreign large-scale target manufacturers, and its utilization rate can reach 70% in theory, which is much higher than the 20%-30% use of planar targets. Rate. [0003] Tubular molybdenum-niobium alloy sputtering target (Mo:Nb=90:10at%) is difficult to be p...

Claims

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Application Information

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IPC IPC(8): C23C14/34B22F3/04B22F3/15B22F3/24B22F1/00B22F5/00
CPCC23C14/3414B22F3/04B22F3/15B22F3/24B22F5/00B22F2003/248B22F2999/00B22F1/05B22F2201/20
Inventor 李培林文宏福
Owner 广东欧莱高新材料股份有限公司