Preparation method of tubular niobium target for magnetron sputtering

A magnetron sputtering and tubular technology, which is applied in the field of preparation of tubular niobium targets for magnetron sputtering, can solve the problems of high equipment requirements, affecting the purity of niobium processing residues, and the influence of the outer diameter of tubular targets. Achieve the effect of ensuring dimensional accuracy and surface quality, avoiding uneven blank size, and ensuring organizational performance characteristics

Inactive Publication Date: 2012-11-28
西安方科新材料科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Usually, the niobium tube target prepared by the casting method has coarse grains, low tube target strength, complex subsequent processing procedures and low film formation rate; although the niobium plate coiled tube welding process is simple and the yield is high, this method is due to the weld seam Existence, resulting in uneven structure of the niobium tube target, will have a serious impact on the uniformity of the coating; the centrifugal casting method is a near-forming technology, the method is simple, and there is less follow-up processing, but it has high requirements for equipment, and it is difficult to produce large-size niobium tube targets and process them. Large-scale industrial production; it is difficult to prepare a thick-walled tube target by electroplating or thermal spraying niobium metal on the support tube, and the wall thickness of the tube target is an important factor to improve the utilization rate of the target
[0005] The invention patent with the publication number CN 102489951A published on June 13, 2012 provides a method for preparing a niobium tubular target for sputtering. The purpose is to provide anti-oxidation protection for the niobium tube billet, but during the extrusion process, the sheath is likely to cause uneven deformation and clogging within the range of about 400mm at the outlet end of the tube billet, which has a serious impact on the outer diameter of the tubular target in this section. Affected or even scrapped; at the same time, the sheath material is difficult to remove in the subsequent process, which seriously affects the purity of niobium processing residues and generates waste
In addition, this method first performs vacuum heat treatment on the extruded niobium tube target, and then performs mechanical processing. After vacuum heat treatment, the strength and hardness of pure metal niobium decrease, and it is difficult to ensure the dimensional accuracy and surface finish of the tubular niobium target during machining.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] Step 1, forging the Nb1 ingot with a diameter of 220 mm and a length of 602 mm prepared by electron beam melting into a cylindrical niobium billet with a diameter of 270 mm at a temperature of 1200 ° C;

[0025] Step 2: Drilling a through hole with a diameter of 50 mm in the center of the cylindrical niobium blank in step 1 to obtain a tubular niobium blank, and then uniformly coating the inner and outer wall surfaces of the tubular niobium blank with an anti-oxidation coating (conventional niobium blanks can be used) Glass protective lubricant, such as glass protective lubricant TLC-8 of Beijing Tianli Chuang Glass Technology Development Co., Ltd.), to prevent the oxidation of the surface of the tubular niobium blank during the subsequent extrusion process;

[0026] Step 3, extruding the tubular niobium billet coated with the anti-oxidation coating in step 2 at an extrusion temperature of 900° C. and an extrusion ratio of 4.1 into a niobium tube billet with an outer dia...

Embodiment 2

[0031] Step 1, forging the Nb1 ingot with a diameter of 260 mm and a length of 560 mm prepared by electron beam melting into a cylindrical niobium billet with a diameter of 275 mm at a temperature of 1000 ° C;

[0032] Step 2: Drilling a through hole with a diameter of 49 mm in the center of the cylindrical niobium blank in step 1 to obtain a tubular niobium blank, and then uniformly coating the inner and outer wall surfaces of the tubular niobium blank with an anti-oxidation coating (conventional niobium blanks can be used) Glass protective lubricant, such as glass protective lubricant FR-35 produced by Beijing Glass Research Institute), to prevent oxidation of the surface of the tubular niobium blank during the subsequent extrusion process;

[0033] Step 3, extruding the tubular niobium billet coated with the anti-oxidation coating in step 2 at an extrusion temperature of 1050° C. and an extrusion ratio of 6.6 into a niobium tube billet with an outer diameter of 140 mm and an...

Embodiment 3

[0038] Step 1, forging the Nb1 ingot with a diameter of 240mm and a length of 548mm prepared by electron beam melting into a cylindrical niobium billet with a diameter of 265mm at a temperature of 1100°C;

[0039] Step 2: Drilling a through hole with a diameter of 51 mm in the center of the cylindrical niobium blank in step 1 to obtain a tubular niobium blank, and then uniformly coating the inner and outer wall surfaces of the tubular niobium blank with an anti-oxidation coating (conventional niobium blanks can be used) Glass protective lubricant, such as glass protective lubricant TB-10 of Beijing Tianli Chuang Glass Technology Development Co., Ltd.), to prevent the oxidation of the surface of the tubular niobium blank during the subsequent extrusion process;

[0040] Step 3, extruding the tubular niobium billet coated with the anti-oxidation coating in step 2 at an extrusion temperature of 980° C. and an extrusion ratio of 7.6 into a niobium tube billet with an outer diameter...

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Abstract

The invention discloses a preparation method of a tubular niobium target for magnetron sputtering. The method comprises the following steps of: forging a niobium casting ingot into a cylindrical niobium blank; drilling a through hole at the center of the cylindrical niobium blank to obtain a tubular niobium blank, and then uniformly coating anti-oxidization coatings on the surfaces of the inner and outer walls of the tubular niobium blank; extruding the tubular niobium blank coated with the anti-oxidization coatings to obtain a niobium tube blank; sequentially carrying out sand spraying, acid washing and machining on the niobium tube blank to obtain a semi-finished product of the tubular niobium target; and carrying out vacuum heat treatment on the semi-finished product of the tubular niobium target to obtain the tubular niobium target for the magnetron sputtering. The tubular niobium target prepared by the method disclosed by the invention has a good structure property; and crystal grains along the wall thickness direction of the target are uniform and can reach the grade of 4-6, the size of the crystal grains is not more than 100 mu m, and the re-crystallization rate of the grains is not less than 90%, so that the uniform consistency of a coating film in the magnetron sputtering is guaranteed.

Description

technical field [0001] The invention belongs to the technical field of sputtering target manufacture, and in particular relates to a method for preparing a tubular niobium target for magnetron sputtering. Background technique [0002] Before 2008, all magnetron sputtering used plate targets, that is, the targets were rectangular plates with a certain thickness in terms of shape. One of the biggest disadvantages of such a target is that the utilization rate of the material is only 25% to 30%. [0003] The use of tubular targets is of particular importance for the coating industry. By assembling a controllable magnet in a seamless tube (tubular target) of a certain size, the surface of the sputtering target has no dead angle, and the self-consumption process of the target surface is relatively uniform, and the material utilization rate can be increased to 70% % or even higher, even if the manufacturing cost of the tubular target itself increases, it will be more than one-thi...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B23P15/00
Inventor 杜永成王歆锐樊雅丽
Owner 西安方科新材料科技有限公司
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