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Preparation method of high hardness zirconium nitride hard coat

A hard coating and zirconium nitride technology, which is applied in the coating, metal material coating process, ion implantation plating, etc., can solve the problems of poor crystallinity of the film layer, unguaranteed service life, and insufficient compactness, etc., to achieve Increased compactness, increased hardness, and increased hardness

Inactive Publication Date: 2010-07-14
XIAMEN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] In recent years, the preparation of ZrN coatings by magnetron sputtering has attracted widespread attention from scholars at home and abroad, and great progress has been made. However, the hardness of ZrN prepared by magnetron sputtering depends on the preparation method, process conditions and test methods. The hardness is concentrated between 15 and 25GPa, but the hardness of about 20GPa cannot work in difficult environments, even cutting under general conditions cannot guarantee its life.
The main reason for the low hardness of the coating is that under normal conditions, the energy of particles obtained by sputtering is only tens of eV, and the diffusion ability of low-energy particles on the surface of the substrate is weak, so the crystallinity of the formed coating layer Poor, insufficient compactness, resulting in lower hardness of the coating

Method used

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  • Preparation method of high hardness zirconium nitride hard coat
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  • Preparation method of high hardness zirconium nitride hard coat

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] 1. Substrate pretreatment: (1) Grinding and polishing: The cemented carbide substrate is subjected to sufficient rough grinding and fine grinding on the 600-mesh and 1200-mesh diamond grinding discs respectively. min, between coarse and fine grinding, the sample should be fully ultrasonically cleaned (ultrasonic cleaning time is 2min) and dried in an oven to remove abrasive dust and oil; after the sample is ground, use W2.5 The diamond polishing powder is used for polishing, and the polishing time is 10 minutes. (2) Ultrasonic cleaning: The polished substrate was cleaned in the following order, acetone ultrasonic cleaning for 5 minutes → absolute ethanol ultrasonic cleaning for 5 minutes → drying for use. (3) Ion source cleaning: Before sputtering deposition, use Hall ion source to clean the substrate, and the pressure of ion cleaning is 2×10 -2 Pa, substrate temperature 300°C, argon flux 10sccm, bias voltage of negative 100V, cathode current and voltage of 29.5A and 1...

Embodiment 2

[0028]1. Substrate pretreatment: (1) Grinding and polishing: Same as Example 1. (2) ultrasonic cleaning: with embodiment 1. (3) ion source cleaning: with embodiment 1.

[0029] 2. Pre-sputtering: same as embodiment 1.

[0030] 3. Sputtering deposition: After the pre-sputtering, argon and nitrogen are introduced, and the flow rate of nitrogen is 20%, the working pressure of deposition is 0.3Pa, the DC power of Zr target is 275W, the sputtering time is 100min, the substrate The temperature is 375°C and the substrate bias is negative 75V. After the deposition is complete, the sample is taken out and stored in a desiccator, pending characterization and analysis. After the deposition is complete, the sample is taken out and stored in a desiccator, pending characterization and analysis.

[0031] image 3 It is the XRD spectrum of the coating, indicating that the prepared coating is a coating with a face-centered cubic structure.

[0032] 4. The chemical composition of the coat...

Embodiment 3

[0035] 1. Substrate pretreatment: (1) Grinding and polishing: Same as Example 1. (2) ultrasonic cleaning: with embodiment 1. (3) ion source cleaning: with embodiment 1.

[0036] 2. Pre-sputtering: same as embodiment 1.

[0037] 3. Sputtering deposition: after the pre-sputtering, argon and nitrogen are introduced, the flow rate of nitrogen is 15%, the working pressure of deposition is 0.5Pa, the DC power of Zr target is 300W, the sputtering time is 110min, the substrate The temperature is 450°C and the substrate bias is negative 75V. After the deposition is complete, the sample is taken out and stored in a desiccator, pending characterization and analysis. After the deposition is complete, the sample is taken out and stored in a desiccator, pending characterization and analysis.

[0038] Figure 4 It is the XRD spectrum of the coating, indicating that the prepared coating is a coating with a face-centered cubic structure. Figure 5 It is the surface SEM morphology of the ...

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Abstract

The invention discloses a preparation method of a high hardness zirconium nitride hard coat and relates to a preparation method of a hard coat, which comprises the following steps: matrix pretreatment: hard alloy matrix is washed and dried after being ground and polished; and the sputter deposition is carried out after the pre-sputtering is performed. A method by adopting magnetic control sputtering method to control the process conditions such as the atmosphere, the matrix temperature, the matrix bias and the like of the sputter deposition so as to prepare the zirconium nitride hard coat on the surface of the hard alloy matrix is adopted to improve the hardness of the zirconium nitride coat. DC power is adopted to perform the magnetic control sputter deposition on the surface of the hard alloy matrix which is mechanically polished, washed by ultrasonic and washed and processed by ion source, the total pressure is controlled at 0.3 to 0.5 Pa, the flow rate of the nitrogen is 15 to 20 percent, DC power of the Zr target is 250 to 300W, the matrix temperature is 300 to 450 DEG C, the matrix bias voltage is minus 50 to 100V, the deposition time is 90 to 120 minutes, and the coat has high hardness of more than 30 GPa.

Description

technical field [0001] The invention relates to a hard coating, in particular to a method for preparing a zirconium nitride hard coating on the surface of a cemented carbide substrate. Background technique [0002] With the popularization of CNC machine tools and machining centers, high-efficiency, high-speed, high-precision cutting has become the main development direction of modern machining technology, and higher requirements have been put forward for the performance of tools. Tool coating is one of the important ways to improve tool performance. By selecting appropriate coating materials and coating preparation methods, the hardness, wear resistance and high temperature oxidation performance of the tool can be improved, thereby increasing the service life of the tool. Among these coated tools, nitride coatings of transition group elements have been widely used in the past two decades due to their high hardness, excellent wear and corrosion resistance and chemical stabil...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C23C14/34C23C14/06C23C14/02C23C14/54
Inventor 王周成祁正兵黄若轩孙鹏朱芳萍
Owner XIAMEN UNIV
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