Effect of Modulation Period on the Properties of Ti-TiN-Zr-ZrN Multilayer Film
Using vacuum cathodic arc deposition technology, three Ti-TiN-Zr-ZrN alternating soft and hard multilayer films with the same thickness and three different modulation periods are deposited on the surface of TC11 titanium alloy. Analyzed and tested the thickness, surface and cross-sectional morphology, hardness, film/base bonding force and sand erosion resistance of the multilayer film with scanning electron microscope, microhardness tester, bond scratch tester and sand erosion tester; The focus is on the influence of the change of the modulation period on the performance of the multilayer film. The results show that as the number of cycles increases, the single modulation cycle becomes thinner, and defects such as metal "droplet" particles in the film are reduced, and a large number of interlayer interfaces are also increased; repeated nucleation between layer interfaces, fine grains It is beneficial to the improvement of the surface finish, density, hardness, bonding force and sand erosion resistance of the multilayer film.
In order to effectively control and reduce the loss caused by solid particles erosion and wear, and to improve the service life of components, scientific and technological workers have conducted various researches in recent years. Among them, coating a layer of erosion-resistant protective coating on the surface of the material is an effective and resource-saving measure. Among many anti-erosion coatings, vapor-deposited nitride hard films have been used in aero engine compressors as early as the 1990s due to their excellent wear resistance, adhesion and surface finish. However, with the development of technology, single-layer nitride hard films (such as TiN) also show some shortcomings. For example, as the thickness increases, the internal stress of the film increases, the bonding force with the substrate becomes poor, and it is easy to fall off. ; At the same time, the corrosion resistance and impact resistance are also poor, and it is difficult to meet the requirements of erosion resistance, so it is necessary to improve the single-layer film system to meet the engineering requirements.
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In order to further improve the performance of the hard film, especially the erosion resistance, many researchers have adopted a multilayer structure to reduce the internal stress, increase the toughness and thickness of the film, and make it have a good bond with the matrix material. Wear resistance, corrosion resistance and impact resistance.
In this paper, vacuum cathodic arc deposition technology is used to install metal Ti and Zr targets at different target positions to prepare Ti-TiN-Zr-ZrN multi-period alternating soft and hard multilayer films. The use of Ti-TiN-Zr-ZrN multi-period soft and hard alternating multilayer film is mainly based on metal nitride ceramic films, which have good corrosion resistance, high hardness and good wear resistance, but poor impact resistance; therefore, in metal nitride ceramics The film is inserted into the soft metal layer, which can greatly improve the toughness of the film and reduce the internal stress of the film. In this way, the change of interlayer composition can be realized by alternating Ti and Zr, which can effectively prevent the growth of columnar crystals, refine the crystal grains, increase the interface, and obtain a multi-layer multilayer with higher hardness, better wear resistance and toughness membrane. The effect of the change of the modulation period on the performance of Ti-TiN-Zr-ZrN multilayer film was studied and compared, in order to optimize an anti-erosion multilayer film with good comprehensive performance.
1. Test method
1. 1. Sample preparation
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The matrix material used in this experiment is mainly TC11 titanium alloy (Ti-6Al-3. 5Mo-1.8Zr) with a size of Φ20 mm × 5 mm, and the surface is polished to a roughness Ra <0.4 μm, and at the same time A polished (100) single crystal Si wafer substrate was used to observe the cross-sectional columnar crystal growth. The cleaning process before sample coating is: 5% metal cleaner solution ultrasonic degreasing→ deionized water rinse→ deionized water ultrasonic→ deionized water rinse→ dehydration→ drying.
The experimental equipment is AS700DTX automatic control twelve arc source cathodic arc coating machine. The furnace can be divided into three rows and can be installed with 12 Φ100 mm circular targets, of which two rows are equipped with a total of 8 Ti targets (purity> 99.9%). The other column is equipped with 4 Zr targets (purity> 99.9%). By adjusting the gas flow and sequentially starting the Ti target and Zr target, deposit Ti-TiN-Zr-ZrN multilayer film, the thickness of Ti-TiN layer and Zr-ZrN layer The ratio is 1:1, and the ratio of the metal layer to the metal nitride layer is 1:6. Taking the Ti-TiNZr-ZrN four-layer structure as a cycle, while keeping the total thickness of the multilayer film with different modulation cycles at the same level, the deposition time of each cycle is controlled by a computer program, and the deposition time is 3, 12 and 24 cycles respectively.的multilayer film.
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The gas used in the test is 99.999% high purity nitrogen and argon. Before film deposition, ion bombardment cleaning was performed with -1000 V bias for 30 min. The main deposition parameters: deposition temperature: 300 ~ 350 ℃, bias voltage: -100 ~ -150 V, N2 pressure: 0.5 ~ 1.0 Pa, target current: 80 ~ 100 A.
1.2, test method
Use Nova NanoSEM 430 ultra-high resolution field emission scanning electron microscope (SEM) to observe the surface and cross-sectional morphology of the film. Use MH-5D hardness tester to measure the Vickers microhardness of the film, the load is 25g, and the holding time is 15s. PHI-700 nano-scanning Auger electron spectroscopy (AES) was used to analyze the depth distribution of film composition. The HH-3000 film bond strength scratch tester is used to test the film/base bond strength. The scratch test uses a maximum load of 100 N, a loading speed of 100 N/min, and a scratch speed of 5 mm/min. The anti-erosion performance is carried out by AS600-special sandblasting tester according to ASTM G76-05 standard, using angular corundum (Al2O3) sand, the size of sand is about 55μm, the sand rate is 30± 2m/s, and the sand feeding rate is about 2 ± 0.5 g/min, using 30°± 2° and 90°± 2° to test the scouring angle of attack.
3. Conclusion
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Using vacuum cathodic arc ion plating technology, 3 kinds of Ti-TiN-Zr-ZrN multi-period alternating soft and hard multilayer films with different modulation periods are prepared on the surface of TC11 substrate. The performance of the multilayer film changes with the modulation period as follows:
(1) Under the condition that the total thickness of the multilayer film is equivalent, as the number of cycles increases, the thickness of each modulation cycle becomes thinner, and the defects such as metal "droplet" particles in the film layer are reduced and smaller, which is beneficial to the surface of the multilayer film Improved finish and flatness.
(2) With the increase in the number of cycles, a large number of interlayer interfaces are increased, and the nucleation between the interfaces of each layer is repeated, so that the grains are refined and the "defects" are reduced, which is conducive to the density, hardness and bonding force of the film. improve.
(3) As the number of cycles increases, the sand erosion resistance of the multilayer film is also improved; at the same time, the erosion resistance of the multilayer film at an angle of attack of 30° is significantly better than that of the angle of attack of 90°.
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.