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Method for preparing niobium sputtering target

A sputtering target material and preparation process technology, applied in sputtering plating, metal material coating process, ion implantation plating, etc., can solve the problem of poor grain size uniform texture formation, product quality and Yield rate is not easy to control and other problems, to achieve the effect of solving the problem of grain uniformity and texture, fast film forming speed, and fine grain

Active Publication Date: 2010-03-03
西安诺博尔稀贵金属材料股份有限公司
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003]At present, in order to prepare niobium sputtering targets that meet the performance requirements, forging equipment is usually used to open the billet by combining upsetting and drawing to achieve the broken cast state Organization, the purpose of increasing the grain size of the finished product, but this method is not good for the uniformity of the grain size and the formation of the [111] texture, and the product quality and yield are not easy to control during the production process

Method used

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  • Method for preparing niobium sputtering target

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Effect test

Embodiment 1

[0016] Melt a niobium ingot with a three-time electron beam with a specification of Φ330×600mm, heat it in an electric furnace to 700°C, keep it warm for 4 hours, heat it to 1100°C in an induction furnace after being out of the furnace, and extrude it into a horizontal extrusion machine to Φ120×L . Blanking to get Φ120×240mm niobium billet, heated to 500°C in an electric furnace, heat preservation for 1h, upsetting and forging on a 3T electro-hydraulic hammer to form a slab ≠60×150×300, and the single-pass processing rate of the first two hammers are greater than 30%. Then through rolling, 900°C, 2h intermediate annealing, 850°C, 1.5h finished annealing, wire cutting and other processes to obtain a finished niobium target ≠20×150×400. The grains of this niobium target are uniform and fine, the fine-grained area is 8.5, the coarse-grained area is 7, and the total amount of [111] texture reached 75% as measured by EBSD.

Embodiment 2

[0018] Melt a niobium ingot with a triple electron beam with a specification of Φ320×450mm, heat it in an electric furnace to 700°C, keep it warm for 4 hours, heat it to 950°C in an induction furnace after being out of the furnace, and then press it into a horizontal extrusion machine to extrude to Φ110×L . Blanking to get Φ110×215mm niobium billet, heated to 600°C in an electric furnace, heat preservation for 1h, upsetting and forging on a 3T electro-hydraulic hammer to form a slab of ≠45×130×350, wherein the single-pass processing rate of the first two hammers are greater than 30%. Then through rolling, 900°C, 2h intermediate annealing, 900°C, 1.5h finished annealing, wire cutting and other processes to obtain finished niobium target ≠6×130×700. The grains of the niobium target are uniform and fine, the fine-grained area is 8.5, and the coarse-grained area is 7.5. The total amount of [111] texture reached 90% as measured by EBSD.

Embodiment 3

[0020] Melt a niobium ingot with a three-time electron beam with a specification of Φ320×500mm, heat it in an electric furnace to 700°C, keep it warm for 4 hours, heat it to 1000°C in an induction furnace after being out of the furnace, and extrude it into a horizontal extrusion machine to Φ130×L . The niobium billet of Φ130×220mm is obtained by blanking, heated to 700°C in an electric furnace, kept for 1 hour, upsetting and forging on a 3T electro-hydraulic hammer to form a slab of ≠40×450×160, and the single-pass processing rate of the first three hammers is are greater than 30%. Then through rolling, 900°C, 2h intermediate annealing, 900°C, 1.5h finished annealing, wire cutting and other processes to obtain the finished niobium target of Φ450×8. The grains of the niobium target are uniform and fine, the fine-grained area is grade 7, and the coarse-grained area is grade 8.5. The total amount of [111] texture reached 72% as measured by EBSD.

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Abstract

The invention relates to a method for preparing niobium sputtering target, which is characterized in that the preparation process sequentially comprises the steps: (1) extruding a niobium ingot with the diameter of 300-330mm to be a niobium rod with the diameter of 100-150mm at the temperature of 900-1100 DEG C, and controlling the extrusion ratio to be more than 7; (2) after heating the niobium rod to be 500-700 DEG C for homeothermy, and upsetting and reshaping the niobium rod to be a plate blank by an air hammer, wherein controlling the processing rate of the previous two times of upsettingto be more than or equal to 30%; (3) carrying out intermediate annealing on the plate blank with the annealing temperature of 900-1100 DEG C and the heat preservation time of 1-2h; (4) after annealing, rolling the plate blank, and controlling the single processing rate of the previous two times of upsetting to be more than 35% and the subsequent rolling processing rate to be more than 20%; and (5) annealing the rolled finished product. The method adopts high temperature extrusion with high processing rate, so as to lead the niobium rod to have dynamic recrystallization when in the extruding process and ensure the crystalline grains to be fully ground, so that the difference between the sizes of the crystalline grains at the core part and the edge of a cast ingot can be reduced, the orientation of the crystalline grains can be ensured to be consistent, and more than 70% (111) type texture can be obtained.

Description

technical field [0001] A method for preparing a niobium sputtering target, in particular to a method for preparing a niobium sputtering target with fine uniform grains and a high content of [111] type texture. Background technique [0002] Niobium sputtering target is an important raw material for the preparation of thin film materials. It is widely used in high-end industries such as optics, electronics, and information, such as shipbuilding, chemical industry, liquid crystal display (LCD), industrial glass, camera lenses, integrated circuits, information storage, and solar energy. And coating industry such as heat-resistant, corrosion-resistant and high-conductivity. With the continuous update and supplementation of sputtering equipment, the demand for target materials and quality requirements are increasing. In order to obtain uniform film thickness and faster sputtering speed, niobium targets are required to have high purity, uniform and fine grains. And strong [111] ty...

Claims

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Application Information

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IPC IPC(8): C23C14/34C23C14/14C22F1/18C21D1/26
Inventor 宜楠张锟宇孙毅王飞李俊于乐庆赵鸿磊
Owner 西安诺博尔稀贵金属材料股份有限公司
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