Structure and properties of TiCN thin films prepared by co-sputtering graphite target and titanium target

Prepare TiCN film on M2 high-speed steel substrate by co-sputtering graphite target and titanium target in a mixed atmosphere of nitrogen and argon. Use scanning electron microscope and X-ray diffractometer to analyze the structure and structure of TiCN film, and use nanoindenter The hardness of the TiCN film was tested, and the indentation method and the scratch method were used to evaluate the bond between the film and the substrate, and the cutting test of the TiCN film tap was performed to investigate the durability of the TiCN film. The results show that the C atoms in the TiCN film exist in the form of solid solution in the TiN lattice. The orientation of the TiCN film on the (111) crystal plane is significantly weaker than that of the TiN film. The fracture of the TiCN film is a long block structure, and its lateral size is larger than that of TiN. The film is small, and the surface of the TiCN film is uneven. The bonding force between the TiCN film and the substrate is about 40N. C atoms have solid solution strengthening and fine grain strengthening effects in the TiCN film. The hardness of the TiCN film is increased from 20.3 to 33.4GPa of the TiN film. TiCN film has good anti-friction performance. The service life of TiCN film taps when tapping 40Cr is significantly longer than that of TiN film taps and uncoated taps.

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The rapid development of contemporary cutting technology puts forward higher requirements on the materials and performance of the cutting tools, and dry and high-speed cutting have become the direction of the development of cutting tools. Depositing a hard film on the surface of the tool has become one of the feasible ways to improve and enhance the performance of the tool. TiN, TiC, TiCN and TiAlN hard films are several kinds of tool surface protective layers that appeared earlier, and are also protective films that are still widely used in the mechanical field. Due to its high hardness and low coefficient of friction, TiCN film has very good wear resistance, so it is widely used in tools, molds and wear-resistant parts. The preparation method of TiCN film is mainly vapor deposition method, including chemical vapor deposition (CVD) method and physical vapor deposition (PVD) method. The temperature in the furnace in the process of preparing thin films by CVD method is usually higher than 850℃. Even the medium temperature chemical vapor deposition technology (MT-CVD), its working temperature is generally around 600℃, which exceeds the tempering temperature of steel molds and parts. Therefore, this method is not suitable for coating on steel substrates. The working temperature of PVD film preparation is generally below 500 ℃, which can meet the coating requirements of steel substrates.

At present, the PVD method mostly uses CH4 or C2H2 as the C source to prepare TiCN films. During the preparation process, the TiCN films with different element content ratios and different properties can be obtained by adjusting the gas flow ratio. However, the problem with this method is that excessive carbon source gas will cause serious pollution to the internal structure of the furnace body of the coating machine, and the loose carbon layer remaining on the furnace wall will be released during the next coating, which will interfere with the deposition atmosphere of the film. Continuous production is unfavorable and often leads to instability of the performance of thin film workpieces in industrial production.

The use of solid C source to prepare TiCN film can greatly reduce or avoid pollution to the furnace body. Reactive magnetron sputtering is one of the main technologies of the PVD method. There are no large particles on the surface of the coating prepared by this method, and the surface quality of the coating is good. TiCN thin films can be prepared on a steel substrate. Guojun Zhang et al. prepared TiCN films by sputtering a graphite target and a titanium target in a mixed atmosphere of nitrogen and argon. They pointed out that as the sputtering power of the graphite target increases, the deposition efficiency increases, and the results are obtained in the same time. The total thickness of the film and the modulation period both increase; as the power of the sputtering target increases, the structure of the TiCN film changes, the (111) and (220) crystal plane orientations gradually weaken, and the hardness of the TiCN film first increases and then decreases, reaching the highest The hardness is above 40GPa; the friction coefficient of the TiCN film decreases with the increase of the sputtering power of the graphite target, and finally remains at about 0.2. Xu Junhua et al. used magnetron sputtering technology to prepare TiCN films using solid carbon sources. The effect of graphite sputtering target power on the structure and hardness of TiCN films obtained in this study is basically the same as that of graphite target sputtering current. However, the Vacuum Technology Network (http://www.chvacuum.com/) believes that none of the above research reports has tested the composition of the TiCN film, and it is not clear about the carbon content in the TiCN film prepared by using a solid carbon source, and it has not been corrected. The bonding strength between TiCN film and substrate is analyzed.

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In this paper, the RZP-800 intermediate frequency reactive magnetron sputtering coating machine developed by Sichuan University is used. A graphite target is used as a carbon source instead of CH4 or C2H2. TiCN is prepared by co-sputtering a graphite target and a titanium target in a mixed atmosphere of nitrogen and argon. The composition, structure, hardness and bonding strength of the TiCN film obtained by the preparation method are analyzed and studied. At the same time, the actual application of the TiCN film deposited on the surface of the high-speed steel wire cone by this method is investigated.

Choose M2 high-speed steel as the base material, the sample size is 6mm×6mm×10mm, and prepare several Φ10mm taps of the same material for cutting test. The sputtering target material is a pair of titanium metal target (purity 99.99%) and graphite target (purity 99.99%), and the two targets (4 targets) are arranged alternately and evenly on the inner wall of the coating chamber. Before coating, the surface of the sample is polished to remove the macroscopic scratches visible to the naked eye, and polished to a mirror surface. Then the tap and the sample are sandblasted to remove the contamination of the superficial layer. After ultrasonic cleaning, it is blown dry and loaded into the furnace. Vacuum to 9.0× 10-3 Pa, preheat the workpiece for 60 minutes, and then use the effect of argon ion bombardment to etch and clean the substrate for 30 minutes under a negative bias. In order to improve the bonding strength between the film and the substrate, the Ti metal block in the evaporation crucible deposits a layer of Ti metal transition layer on the substrate. Finally, the graphite target and titanium target were co-sputtered to prepare TiCN thin films under the pressure of 4.5×10-1 Pa for 3h. After the coating is finished, cool for 1 hour and take out the sample.

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S-4800 (Hitachi, Japan) scanning electron microscope (SEM) was used to observe the fracture structure and surface morphology of the TiCN film, and the element content of the film was analyzed with the X-ray energy spectrometer (EDS) attached to the instrument. X′ Pert Pro (Philips, Holland) X-ray diffraction (XRD) instrument was used to analyze the phase composition and grain size of the coating. Nano Indenter XP test system (Agilent, America) was used to analyze the hardness and elastic modulus of the coating. At the same time, the indentation method and the scratch method are used to evaluate the bonding strength of the film and the substrate. The indentation method uses the HR-150A Rockwell hardness tester with a load of 150kg; the scratch method uses the HH-3000 scratch tester with a termination load of 100N. A Z5135 vertical drilling machine was used to conduct a cutting test on the tap. The spindle speed of the drilling machine was 530r/min, the tapped material was 40Cr quenched and tempered steel, and the hardness after quenching and tempering was HRC29-32.

Using a solid carbon source, a graphite target and a titanium target were co-sputtered by reactive magnetron sputtering technology to prepare TiCN films on high-speed steel substrates, and the structure and properties of the obtained TiCN films were systematically analyzed. The conclusions are as follows:

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(1) The fracture of the TiCN film is a long block structure that grows perpendicular to the interface. The uneven structure on the surface of the TiCN film is weaker than that of the TiN film, while the surface of the TiCN film has more microparticles; the TiCN film forms a TiN-based solid solution , The addition of C atoms significantly reduces the diffraction peak of the film on the (111) crystal plane.

(2) Due to the solid solution strengthening and fine-grain strengthening of C atoms, the hardness of TiCN film is significantly higher than that of TiN film, and the hardness of TiCN film is 33.4GPa; after the Ti transition layer is bottomed, the TiCN film and TiN film are combined with M2 high speed The bonding strength of the steel matrix is not much different, both are about 40N.

(3) The wear form of TiCN film is mainly abrasive wear. During friction and wear, a carbon transfer film is formed on the surface of the film. This film plays a role of solid lubrication and anti-friction. When tapping 40Cr material, the service life of TiCN film taps is significantly improved. It is 3 times and 1.6 times that of non-film tap and TiN film tap respectively.

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.