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Method for preparing zirconium wolframic acid-copper gradient composite film

A composite film, zirconium tungstate technology, used in ion implantation plating, metal material coating process, coating and other directions

Inactive Publication Date: 2008-02-06
JIANGSU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Zirconium tungstate-copper composite films were prepared by using a microwave ECR plasma-enhanced deposition system, magnetron sputtering and subsequent reduction heat treatment. So far, there is no report or patent literature to refer to

Method used

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  • Method for preparing zirconium wolframic acid-copper gradient composite film

Examples

Experimental program
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Effect test

Embodiment 1

[0038] (1) Preparation of magnetron sputtering target

[0039] ZrO 2 and WO 3 Weigh according to the molar ratio of 1:2, add distilled water for stirring, and dry by ball milling. Screen the dried mixture, add binder PVA accounting for 5% of the total weight of the oxide, mix evenly, and press it into a target at 80Mpa; place the target in a high-temperature sintering furnace for sintering, at 1200°C Keep warm for more than half an hour to make a target; take out the target and grind it with sandpaper to ensure that the top and bottom of the target are flat; the copper target is a commercially available target.

[0040] (2) Surface activation treatment of single crystal Si(100) substrate

[0041] Immerse the silicon wafer in ethanol and ultrasonically clean it for 10 minutes; then soak it in a solution of hydrogen peroxide: concentrated sulfuric acid = 1:2 for 10 minutes; take it out and immerse it in a beaker containing a mixture of HF: deionized water = 1:10 for 20 second...

Embodiment 2

[0048] (1) Preparation of magnetron sputtering target

[0049] ZrO 2 and WO 3 Weigh according to the molar ratio of 1:2, add distilled water for stirring, and dry by ball milling. Screen the dried mixture, add binder PVA accounting for 4% of the total weight of the oxide, mix evenly, and press it into a target material under 60Mpa; sinter the target material, and keep it at 1150°C for more than half an hour. The target is made; the target is taken out and polished to ensure that the upper and lower sides of the target are flat; the copper target is selected from commercially available targets.

[0050] (2) Surface activation treatment of single crystal Si(100) substrate

[0051] Immerse the silicon wafer in ethanol and ultrasonically clean it for 10 minutes; then soak it in a solution of hydrogen peroxide: concentrated sulfuric acid = 1:2 for 12 minutes; take it out and immerse it in a beaker filled with a mixture of HF: deionized water = 1:10 for 30 seconds; Blow dry with...

Embodiment 3

[0058] (1) Preparation of magnetron sputtering target

[0059] ZrO 2 and WO 3 Weigh according to the molar ratio of 1:2, add distilled water for stirring, and dry by ball milling. Screen the dried mixture, add binder PVA accounting for 10% of the total weight of the oxide, mix evenly, and press it into a target material at 100Mpa; sinter the target material, and heat it at 1250°C for more than half an hour. The target is made; the target is taken out and polished to ensure that the upper and lower sides of the target are flat; the copper target is selected from commercially available targets.

[0060] (2) Surface activation treatment of single crystal Si(100) substrate

[0061] Immerse the silicon wafer in ethanol and ultrasonically clean it for 15 minutes; then soak it in a solution of hydrogen peroxide: concentrated sulfuric acid = 1:2 for 15 minutes; take it out and immerse it in a beaker filled with a mixture of HF: deionized water = 1:10 for 20 seconds; Blow dry with ...

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Abstract

A process for preparing zirconium tungstate-copper gradient composite films relates to the technical field of composite film preparation, and comprises: preparing magnetic-control sputtering targets firstly; then conducting surface activation treatment on a mono-crystal Si substrate with the conventional technology; placing the composite oxide target, copper target and the silicon slice respectively into a main sputtering room and a sample-introducing room; vacuumizing the main sputtering room and the sample introducing room; pre-sputtering on the oxide target for clearing away impurities on the surface; adjusting the volume ratio of argon to oxygen to be between zero and one, the distance between the base material and the target to be 5 to 15cm, and the sputtering power to be 130 to be 250W for striking sputtering; setting the sputtering power of the composite oxide plated target to be 200 to 280W and of the Cu target to be 50 to 70W; for every hour, increasing the sputtering power of the Cu target by 10 to 20W while decreasing the sputtering power of the composite oxide target by 20 to 50W; taking the sample out from the main sputtering room after sputtering; conducting heat treatment on the film. Thereby a ZrW2O8 / Cu gradient composite film is obtained. The present invention has the advantages of simple process, easy implementation, short synthesis time and low post heat-treatment temperature.

Description

technical field [0001] The patent of this invention relates to a preparation method of a composite film, specifically ZrW 2 o 8 / Cu gradient composite film and the preparation method of radio frequency magnetron co-sputtering + subsequent reduction heat treatment, through the implementation of this method, a gradient function film with high electrical conductivity, high thermal conductivity, continuous change of thermal expansion coefficient, and gentle transition of interlayer stress can be obtained. Background technique [0002] In the field of electronics, the interconnection of devices in integrated circuits is an important process step, and there are strict requirements for interconnection conductive materials. A typical wiring metal is Al (doped with Si or Cu). However, with the increase of VLSI (very large integrated circuit) integration, the further reduction of wiring line size, electromigration phenomenon of aluminum wiring (causing short circuit and open circuit...

Claims

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Application Information

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IPC IPC(8): C23C14/35C23C14/06C23C14/54C23C14/58
Inventor 严学华程晓农宋娟赵国平
Owner JIANGSU UNIV
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