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Preparation method for low-stress compact coating layer

A low-stress, coating technology, which is applied in the preparation of thick/ultra-thick coatings and the preparation of low-stress dense coatings, can solve the problems of poor mechanical properties of coatings, degradation of substrate properties, stress relief, etc. Stress, low equipment requirements, high compactness effect

Inactive Publication Date: 2018-08-17
SOUTHEAST UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, for ultra-low negative bias voltage, insufficient ion bombardment will lead to loose coating, the annealing method may not be able to relieve the stress in time or the performance of the substrate may be deteriorated due to excessive annealing, and the mechanical properties of the coating are often poor through gradient or multi-layer design.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0016] Example 1: Preparation of low-stress dense TiAlN coating

[0017] Ti 6 Al 4 V samples (workpieces) are cleaned and put into a vacuum chamber to evacuate to 6X10 -4 Pa. The inert gas argon was introduced, the bias voltage was -800V to -1000V, and the surface of the sample was etched for 20 minutes. The inert gas argon is introduced, and the intermediate layer Ti, etc. is sputtered, with a thickness of about 200nm. Argon, krypton, xenon and nitrogen are introduced, the content of argon in the inert gas is 1%, the content of krypton in the inert gas is 1%, the content of xenon in the inert gas is 98%, nitrogen is mixed The content in the gas is 7%, and the TiAl target DC sputtering power density is 10W / cm 2 , the ionization rate is 10%, the bias voltage is -50V, the deposition time is 10 hours, the thickness of the obtained TiAlN coating is 20um, the density is 99%, and the stress is -100MPa.

Embodiment 2

[0018] Example 2: Preparation of low-stress dense TiAlN coating

[0019] Ti 6 Al 4 The V sample is cleaned and put into a vacuum chamber to evacuate to 6X10 -4 Pa. The inert gas argon was introduced, the bias voltage was -800V to -1000V, and the surface of the sample was etched for 20 minutes. The inert gas argon is introduced, and the intermediate layer Ti, etc. is sputtered, with a thickness of about 200nm. Incorporate argon, krypton, xenon and nitrogen, the content of argon in the inert gas is 1%, the content of krypton in the inert gas is 20%, the content of xenon in the inert gas is 69%, nitrogen in the mixed gas The content is 7%, and the TiAl target DC sputtering power density is 10W / cm 2 , the ionization rate is 10%, the bias voltage is -50V, the deposition time is 10 hours, the thickness of the obtained TiAlN coating is 20um, the density is 98%, and the stress is -800MPa.

Embodiment 3

[0020] Example 3: Preparation of low-stress dense TiAlN coating

[0021] Ti 6 Al 4 The V matrix sample is cleaned and put into a vacuum chamber to evacuate to 6X10 -4 Pa. The inert gas argon was introduced, the bias voltage was -800V to -1000V, and the surface of the sample was etched for 20 minutes. The inert gas argon is introduced, and the intermediate layer Ti, etc. is sputtered, with a thickness of about 200nm. Incorporate argon, krypton, xenon and nitrogen, the content of argon in the inert gas is 20%, the content of krypton in the inert gas is 1%, the content of xenon in the inert gas is 69%, nitrogen in the mixed gas The content is 7%, and the TiAl target DC sputtering power density is 10W / cm 2 , the ionization rate is 10%, the bias voltage is -50V, the deposition time is 10 hours, the thickness of the obtained TiAlN coating is 20um, the density is 99%, and the stress is -500MPa.

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PUM

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Abstract

The invention discloses a preparation method for a low-stress compact coating layer. The preparation method comprises the following steps: step 1, thoroughly cleaning a workpiece, placing the workpiece in a vacuum chamber and vacuumizing until the vacuum degree is more than 6*10<-4>Pa, charging inert gas argon, controlling a bias voltage to be -800V to -1000V, and etching the surface of the workpiece for 10 minutes to 60 minutes; step 2, charging the inert gas argon, sputtering an interlayer Ti or Cr with a thickness of 100nm to 500nm; and step 3, charging the mixed gas of inert gases argon and krypton, argon and xenon or argon, krypton and xenon, and sputtering the needed deposited coating layer. In a sputtering deposition process, a working gas is the mixed gas of argon and krypton, argon and xenon or argon, krypton and xenon, and the reasonable deposition bias voltage is controlled, so that the stress level of the coating layer is controlled. Relative to the traditional coating layer, the pressure stress is lower under the condition of obtaining a compact structure; and the preparation method is applicable to the application fields of coating layers with high binding performancerequirements and large thicknesses.

Description

technical field [0001] The invention belongs to the field of vacuum deposition coating preparation technology, in particular to a preparation method of low-stress dense coating, which can be used for the preparation of thick / ultra-thick coating. Background technique [0002] At present, the thickness of dense hard coatings prepared by magnetron sputtering generally does not exceed 10um. The main reason is that excessive compressive stress deteriorates the bonding performance of the thick coating / substrate, and also causes the coating itself to break and fail under load. . During the deposition process, ions bombard the coating, which induces interstitial defects in the coating, which is the main cause of compressive stress. The increase of coating thickness can greatly improve the bearing capacity of the substrate surface, and at the same time significantly improve the wear life. Therefore, thick hard coatings (thickness greater than 10um) have wider industrial application ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C23C14/35C23C14/06C23C14/08C23C14/16
CPCC23C14/35C23C14/0036C23C14/0635C23C14/0641C23C14/08C23C14/165
Inventor 张旭海陈龙郑云西肖静才曾宇乔朱奎季宝荣卢倩文杨志李娟蒋建清
Owner SOUTHEAST UNIV
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