Measurement and analysis of the adhesion force of TiN/TiCrN/TiCrAlN composite film
A scratch test was carried out on the TiN/TiCrN/TiCrAlN composite film prepared by multi-arc ion plating with a scratch tester. The surface morphology of the scratch was observed and analyzed by a metallurgical microscope, and the film-base bonding force of the composite film was comprehensively determined. The results show that the failure mode of the film is peripheral peeling; a single acoustic signal curve cannot accurately determine the critical load of film failure, and a comprehensive determination of the acoustic signal curve and the scratch morphology is required.
The good combination of the film and the substrate is the basic premise to ensure that the film meets the mechanical, physical and chemical performance of the film. The quality of the combination is a key indicator for evaluating the quality of the film. Therefore, the measurement of the interface bonding properties of thin film materials has very important significance in practical applications.
At present, various measurement methods such as indentation method, scratch method, stretching method, bulging method, bending method, and laser method are used to determine the bonding performance between the film and the substrate. However, due to the complexity and diversity of the membrane/substrate system, no method has yet been applied to any membrane/substrate system.
The scratch method is usually suitable for the film with a thickness of 0.1-20μm, and it has practical significance only when the shear strength of the film is greater than the bonding strength of the film/substrate interface. For this type of film, when the film/base bonding force is measured in the scratch test, failure modes such as breakage and peeling of the film often occur. The Vacuum Technology Network (http://www.chvacuum.com/) believes that the scratch method is a widely used method for measuring the binding force of the membrane base.
There are many types of scratch instruments used in the scratch method. At present, the sound signal emitted when the scratch is measured is the mainstream. However, the defects of the film or the substrate interfere with the acoustic signal, which makes it difficult to accurately match the failure of the film and the acoustic signal during scratching. Especially for the film prepared by multi-arc ion plating, the presence of metal droplets is inevitable. , Its acoustic signal is more susceptible to interference. How to accurately determine the critical load has become a key issue in the determination of membrane-base binding force by the scratch method. To this end, many scholars use other direct or indirect information, combined with acoustic signals to accurately determine the critical value of film failure.
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In this study, the TiN/TiCrN/TiCrAlN composite film prepared by multi-arc ion plating was used as the object. According to the acoustic signal data, friction data, and friction coefficient data collected by the scratch instrument, the scratch morphology was observed and analyzed under a metallurgical microscope. Comprehensive determination of membrane-base binding force provides an accurate and credible criterion for the determination of membrane-base binding force.
1. Experiment
1.1, sample preparation
The coating equipment used for sample preparation is the TRX-3(A) multifunctional vacuum ion coating machine developed by Beijing Tianruixing Vacuum Technology Development Co., Ltd. Using Ti, Al, Cr three metal single target materials, TiN, TiCrN, TiCrAlN thin films are plated layer by layer on the surface of high-speed steel (W18Cr4V). The substrate sample to be plated is polished, degreasing, ultrasonic cleaning and dehydration treatment. When the background vacuum of the coating chamber reaches 3.0× 10-3 Pa and the temperature reaches 220℃, the reaction gas N2 is introduced, and the N2 pressure is 6.0× ; 10-1 Pa. The pre-bombardment cleaning was carried out at -600V bias for 5 minutes, and then the coating experiment was carried out at -200V bias. The target current and deposition time are shown in Table 1.
Table 1 Target current and deposition time
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Measurement and analysis of the adhesion force of TiN/TiCrN/TiCrAlN composite film
1.2, scratch experiment
In this study, the MFT-4000 multifunctional material surface performance tester (hereinafter referred to as the scratch tester) developed and designed by the Lanzhou Institute of Chemical Physics, Chinese Academy of Sciences (hereinafter referred to as the scratch tester) was used to conduct scratch experiments on the samples. The scratch tester can collect acoustic signals during the test. And tangential friction, friction coefficient.
Fix the sample to be tested horizontally on the stage fixture, randomly select three positions on the surface of the sample, select appropriate measurement parameters, and conduct a scratch experiment. The selection parameters of the scratch instrument are shown in Table 2. The curve of acoustic signal, friction force and friction coefficient obtained by the scratch tester when completing a scratch is shown in (a).
Table 2 Scratch tester parameters
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Measurement and analysis of the adhesion force of TiN/TiCrN/TiCrAlN composite film
3. Conclusion
Through comprehensive analysis of the scratch morphology and scratch gauge curve of the TiN/TiCrN/TiCrAlN composite film plated by the multi-arc ion plating method, the following conclusions are drawn:
1. The acoustic signal curve alone cannot accurately determine the film-base bonding force. The acoustic signal curve and the scratch morphology must be combined to comprehensively determine the critical value of film failure.
2. Judging by the scratches on the surface of the film, the failure mode of the film is peripheral peeling.
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Founded in 2015,Zunhua Baorui Titanium Equipment Co.,Ltd. is a manufacturer specializing in pvd vacuum ion coating equipment. The company’s products mainly include large plate coating machine, large tube collating machine, tool coating machine and LOW-E glass production line. Mr.Wang baijiang ,general manager of the company ,has been engaged in vacuum coating industry for more than 30 years. He continuously improve production technology, improve product performance and devote himself to provide customers with better product experience and higher production efficiency.