Multi-arc ion plating technology is used to synthesize TiN/Ti multilayer films with nanometer modulation period under different deposition parameters. X-ray diffractometer (XRD), scanning electron microscope (SEM), XP-2 step meter, XP nanoindenter, X-ray energy spectrometer (EDS) were used to study the effect of modulation period on the microstructure of TiN/Ti nano multilayer films. The influence of structure, surface morphology and mechanical properties. The results show that the film layer is composed of TiN and Ti alternately, there are no other impurity phases, and the TiN film grows preferentially along the (111) densely packed surface with a face-centered cubic structure; the TiN/Ti multilayer film has a dense, smooth appearance and uniform golden color. As the modulation period decreases, the number and size of large particles on the surface of the film decrease, and the nitrogen content gradually increases, and the hardness of the film shows an increasing trend.
In recent years, the films prepared by the physical vapor deposition method have high hardness, stable chemical properties, and good friction properties. They are widely used in the fields of cutting tools, molds, various wear-resistant parts, and microelectronics. It is easy to oxidize to form TiO2 at high temperature of ℃, which affects its performance. With the continuous improvement of processing requirements, it is more and more important to study films with better comprehensive properties. People have improved the process, such as: using magnetic filtration to filter large particle droplets, using composite plating methods to optimize film performance, and mixing other metals, such as Al, C, Cr, Zr, etc., these methods have a certain degree of film performance Improvement. According to reports in the literature, the structural characteristics of the materials of the multilayer film and the complex interface conditions between the layers can improve the toughness and crack resistance of the film. But at present, there are few researches on its performance. In this paper, on the basis of TiN coating and multilayer structure, TiN/Ti multilayer film is prepared by multi-arc ion plating method, and the effect of modulation period on its structure and performance is analyzed and studied. influences.
1. Experiment
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The domestic SA-700 6T multi-arc ion plating was used to prepare TiN/Ti multilayer films on high-speed steel substrates, and the effect of different modulation cycles on the mechanical properties of TiN/Ti multilayer films was studied.
The specifications of high-speed steel substrate samples are 10mm×10mm×15mm. First, the substrate samples are polished on No. 600, No. 900, No. 1200, No. 1500, No. 2000 sandpaper in sequence, and then polished with corundum powder on a polishing machine to make the high-speed steel The surface of the substrate is mirror smooth. Before coating, the samples were ultrasonically cleaned with absolute ethanol and acetone for 15 min. After drying, they were placed on the sample holder in the chamber with a target base distance of 300 mm. When working, the pure Ti target is used to deposit the coating, ignite the cathode target arc, and evaporate it with the arc; the vacuum of the deposition chamber is pumped to 5×10-3 Pa below, and Ar gas is introduced for glow and sputter cleaning .
Nano multilayer films have attracted much attention due to their better fracture toughness and super-hard supermodel effect. For the nano multilayer film formed by Ti and TiN materials, the sum of the thickness of two adjacent layers is called the modulation period, and the ratio of their thickness is called the modulation ratio. The modulation period is one of the main factors affecting the performance of TiN/Ti multilayer films. Under the condition of a certain total experiment time, the modulation period is inversely proportional to the number of cycles. In the experiment, assuming that the deposition rates of the two films are the same, the ratio of the deposition time of the TiN layer to the Ti layer is 5:1, that is, the nominal modulation ratio is 5:1. In order to prepare multi-layer films with excellent performance, this experiment is designed to deposit 4 sets of samples with different modulation periods under the same nominal modulation ratio. The specific experimental process parameters are shown in Table 1. First, adjust the Ar gas flow and N2 flow to deposit TiN for 50 minutes; adjust the Ar gas flow and gas pressure to deposit Ti for 10 min. The Vacuum Technology Network (http://www.chvacuum.com/) believes that under the same experimental conditions, to ensure that the total experimental time is 60 min and the modulation ratio remains unchanged, the number of cycles is changed by changing the deposition time of TiN and Ti respectively.
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Table 1 Experimental process parameters of TiN/Ti multilayer film
TiN/Ti Multilayer film experimental process parameters
Use X-ray diffractometer (XRD), scanning electron microscope (SEM), XP-2 step meter, XP nanoindenter, X-ray energy spectrometer (EDS) to study the effect of modulation period on the microstructure of TiN/Ti nano multilayer film , Surface morphology and mechanical properties.
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3. Conclusion
(1) The film layer is composed of TiN and Ti, there are no other impurity phases, and the TiN film grows preferentially along the (111) close-packed surface with a face-centered cubic structure.
(2) The appearance of TiN/Ti multilayer film is compact and smooth, and the color is uniform golden yellow. As the modulation period decreases, the number and size of large particles on the surface of the film decrease, and the nitrogen content gradually increases, indicating that Ti and The N2 reaction is gradually full.
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(3) With the decrease of the modulation period, the Vickers hardness shows an increasing trend, indicating that the modulation period has a significant effect on the hardness of the film.
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.