CN113529038A - Preparation method of friction-resistant and corrosion-resistant TiN film - Google Patents
Preparation method of friction-resistant and corrosion-resistant TiN film Download PDFInfo
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- CN113529038A CN113529038A CN202110812568.3A CN202110812568A CN113529038A CN 113529038 A CN113529038 A CN 113529038A CN 202110812568 A CN202110812568 A CN 202110812568A CN 113529038 A CN113529038 A CN 113529038A
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- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 title claims abstract description 54
- 230000007797 corrosion Effects 0.000 title claims abstract description 18
- 238000005260 corrosion Methods 0.000 title claims abstract description 18
- 238000002360 preparation method Methods 0.000 title claims abstract description 13
- 238000000151 deposition Methods 0.000 claims abstract description 38
- 230000008021 deposition Effects 0.000 claims abstract description 31
- 238000000034 method Methods 0.000 claims abstract description 19
- 238000001755 magnetron sputter deposition Methods 0.000 claims abstract description 9
- 238000007733 ion plating Methods 0.000 claims abstract description 6
- 239000010408 film Substances 0.000 claims description 34
- 239000010409 thin film Substances 0.000 claims description 27
- 239000000758 substrate Substances 0.000 claims description 20
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 18
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 10
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 9
- 229910052786 argon Inorganic materials 0.000 claims description 9
- 238000004544 sputter deposition Methods 0.000 claims description 9
- 239000010936 titanium Substances 0.000 claims description 9
- 229910052719 titanium Inorganic materials 0.000 claims description 9
- 239000013077 target material Substances 0.000 claims description 7
- 239000002131 composite material Substances 0.000 claims description 6
- 229910052757 nitrogen Inorganic materials 0.000 claims description 5
- 238000005086 pumping Methods 0.000 claims description 5
- 238000010891 electric arc Methods 0.000 claims description 3
- 239000002356 single layer Substances 0.000 abstract 1
- 230000000052 comparative effect Effects 0.000 description 24
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 16
- 230000010287 polarization Effects 0.000 description 9
- 239000007864 aqueous solution Substances 0.000 description 8
- 239000013078 crystal Substances 0.000 description 8
- 238000005516 engineering process Methods 0.000 description 8
- 239000011780 sodium chloride Substances 0.000 description 8
- 238000002161 passivation Methods 0.000 description 6
- 231100000241 scar Toxicity 0.000 description 6
- 229910045601 alloy Inorganic materials 0.000 description 4
- 239000000956 alloy Substances 0.000 description 4
- 239000011248 coating agent Substances 0.000 description 3
- 238000000576 coating method Methods 0.000 description 3
- 238000005520 cutting process Methods 0.000 description 3
- 230000007547 defect Effects 0.000 description 3
- 238000002474 experimental method Methods 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 229910052751 metal Inorganic materials 0.000 description 3
- 239000002184 metal Substances 0.000 description 3
- 239000000243 solution Substances 0.000 description 3
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 2
- 238000007743 anodising Methods 0.000 description 2
- 230000015556 catabolic process Effects 0.000 description 2
- 238000004140 cleaning Methods 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000011148 porous material Substances 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 1
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- 241000220317 Rosa Species 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000008367 deionised water Substances 0.000 description 1
- 229910021641 deionized water Inorganic materials 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 229910003460 diamond Inorganic materials 0.000 description 1
- 239000010432 diamond Substances 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 238000005530 etching Methods 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229910021421 monocrystalline silicon Inorganic materials 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 239000012466 permeate Substances 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000010935 stainless steel Substances 0.000 description 1
- 229910001220 stainless steel Inorganic materials 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000004506 ultrasonic cleaning Methods 0.000 description 1
Images
Classifications
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/34—Sputtering
- C23C14/35—Sputtering by application of a magnetic field, e.g. magnetron sputtering
- C23C14/352—Sputtering by application of a magnetic field, e.g. magnetron sputtering using more than one target
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/0021—Reactive sputtering or evaporation
- C23C14/0036—Reactive sputtering
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
- C23C14/0641—Nitrides
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/34—Sputtering
- C23C14/3485—Sputtering using pulsed power to the target
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- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Physical Vapour Deposition (AREA)
Abstract
The invention discloses a preparation method of a friction-resistant and corrosion-resistant TiN film, which adopts a deposition method combining multi-arc ion plating and high-power pulse magnetron sputtering to obtain a single-layer TiN film. The method is simple to operate, the friction-resistant and corrosion-resistant TiN film can be obtained by adopting a deposition method combining multi-arc ion plating and high-power pulse magnetron sputtering and only combining two preparation methods with different deposition principles, the method has good repeatability, and the method has important significance for preparing and developing the TiN film with a specific application background.
Description
Technical Field
The invention relates to the technical field of film materials, in particular to a preparation method of a friction-resistant and corrosion-resistant TiN film.
Background
The high-speed development of modern manufacturing industry puts high demands on cutters, and the thin-film material TiN used as a cutter coating not only has high hardness, but also has excellent wear resistance, toughness and good chemical stability. Especially applied to advanced technologies such as high-speed cutting, dry cutting and the like, and the hard film surface coating can realize the performances. The TiN film has the characteristics of high hardness, wear resistance, heat resistance, corrosion resistance and the like. The crystal is a face-centered cubic crystal structure and is formed by mixing metal bonds, covalent bonds and ionic bonds, so that the crystal also has the characteristics of metal crystals and covalent crystals. The TiN film is taken as an ideal metal cutting tool coating, and has excellent properties of high melting point of 2955 ℃, elastic modulus of 616GPa, Vickers hardness of 2245, high-temperature strength, good thermal conductivity and the like, so that the preparation technology becomes the current research hotspot. The single preparation technology has a plurality of defects, such as high deposition rate of ion plating, but large liquid drops and pore defects exist on the surface, which greatly weakens the corrosion resistance; for example, the high-pulse magnetron sputtering has compact surface and low roughness, but has low deposition rate and easy formation of columnar crystals, and chloride ions easily permeate into a substrate in a corrosive environment, so that the application of the thin film material in the fields of modern manufacturing industry, aerospace, electronics and the like is limited to a great extent.
Disclosure of Invention
Aiming at the problems in the prior art, the invention aims to provide a preparation method of a friction-resistant and corrosion-resistant TiN film, which adopts a method of ion plating and high-power pulse magnetron sputtering composite deposition to obtain the required TiN film under the conditions of certain deposition air pressure and sputtering power.
In order to solve the above problems, the present invention adopts the following technical solutions.
A preparation method of a friction-resistant and corrosion-resistant TiN film comprises the following preparation steps:
1) two opposite plane titanium target materials with the same specification and applied to high-power pulse magnetron sputtering are respectively installed on the inner wall of the equipment deposition cavity, and the distance between the plane titanium target materials and the sample table is adjusted to be 100-300 mm;
2) in the deposition chamber of the equipment, the circular arc target is positioned at the horizontal centers of the two plane targets, the included angle between the circular arc target and the plane targets is 60-120 degrees, and the distance between the circular arc target and the sample table is 100-300 mm;
3) placing the cleaned substrate on a rotating stand, and pumping the deposition chamber to a background vacuum (<8 x 10-3 Pa);
4) introducing argon and nitrogen into the deposition chamber, wherein the flow of the argon is 20-100 sccm, the flow of the nitrogen is 20-100 sccm, the deposition pressure is adjusted to be 0.1-1 Pa, a bias power supply is started, and the sample table autorotates at the speed of 3-10 r/min;
5) the planar target adopts a high-power pulse magnetron sputtering mode, the sputtering voltage is adjusted to be 500-1500V, the sputtering current is adjusted to be 100-400A, the sputtering power is 1-5 kW, the pulse width is 50-500 mus, the frequency is 100-500 Hz, and the duty ratio is 1-10%;
6) the circular arc target adopts an arc ion plating deposition mode, the target working current is set to be 50-200A, and the electric arc can stably and uniformly shrink on the surface of the circular arc target by adjusting the magnetic field.
7) Simultaneously starting a power supply to deposit the TiN film;
as a further improvement of the invention, the purity of the titanium target material in the steps 1) and 2) is more than 99.9%.
As a further improvement of the present invention, the base in step 3) is selected from any one of a Si substrate, a SUS 304 substrate, and a cemented carbide substrate.
As a further improvement of the invention, the purity of the argon in the step 4) is more than 99.99%.
As a further improvement of the invention, the sputtering time in the step 7) is 0.5-3 h.
The invention has the advantages of
Compared with the prior art, the invention has the advantages that:
the method is simple to operate, the TiN film with more excellent performance can be obtained only by combining two technologies by adopting a composite technology film deposition method, the method has good repeatability, and the method has important significance for subsequent preparation and development and application of the gradient TiN film.
Drawings
FIG. 1 is a schematic diagram of the chamber structure of the apparatus of the present invention;
FIG. 2 is an SEM photograph of TiN thin films obtained in examples and comparative examples;
FIG. 3 is a graph showing the friction coefficients of TiN thin films obtained in examples and comparative examples;
FIG. 4 is a profile of a wear scar of TiN thin films obtained in examples and comparative examples;
FIG. 5 is a graph showing the friction coefficient and specific wear rate of TiN thin films obtained in examples and comparative examples;
FIG. 6 is an anodic polarization curve of TiN thin films obtained in the examples and the comparative examples in a 3.5 wt.% NaCl aqueous solution;
fig. 7 shows the surface morphology of TiN films obtained in examples and comparative examples after anodizing in 3.5 wt.% NaCl aqueous solution.
Detailed Description
The technical solution in the embodiments of the present invention will be clearly and completely described below with reference to the accompanying drawings in the embodiments of the present invention; it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments, and all other embodiments obtained by those skilled in the art without any inventive work are within the scope of the present invention.
The equipment cavity structure used by the invention is shown in figure 1, a plane A target glow area 2, a circular arc target glow range 3, a circular arc target 4, a rotating frame 5, a cavity inner wall 6, a sample table 7, a plane B target glow area 8 and a plane B target 9.
Example 1
A method for preparing TiN film comprises the following steps:
1) two opposite plane titanium target materials (the purity of the titanium target material is 99.9%) with the same specification and applied to high-power pulse magnetron sputtering are respectively arranged on the inner wall of the deposition cavity of the equipment, and the distance between the two targets is adjusted to be 160 mm;
2) in the deposition chamber of the equipment, the circular arc target is positioned at the horizontal centers of the two plane targets, the included angle between the circular arc target and the plane targets is 90 degrees (the purity of the titanium target is 99.9 percent), and the distance between the plane targets and the circular arc target is 250 mm;
3) the substrate adopts a single crystal Si (100) substrate, an SUS 304 substrate and a hard alloy substrate, wherein the surfaces of the stainless steel and hard alloy substrates are gradually polished by using water abrasive paper (180-300-600-1000-2000), and are polished to a mirror surface state by using diamond abrasive paste (W3), and then the substrate is placed into acetone and alcohol for ultrasonic cleaning twice, each time for 20min, then is washed by deionized water, and finally is dried by using nitrogen;
4) putting cleaned Si (100), SUS 304 and hard alloy into the center of a sample stage in a composite technology deposition chamber, closing a cabin door, starting a rough pumping valve, switching a molecular pump when the deposition chamber is vacuumized to 8Pa, and continuously pumping the deposition chamber to a heating vacuum of 5 x 10 < -2 > Pa;
5) setting the heating temperature to be 150-350 ℃ and the rotating speed of a rotating frame (10r/min), and pumping the deposition cavity to the background vacuum of 8 multiplied by 10 < -3 > Pa;
6) introducing argon (with the purity of 99.999%) into the deposition chamber, adjusting the flow of the argon to 250sccm, setting the deposition pressure to 1.8Pa, setting the negative bias of the rotating frame (700-900V), and performing glow cleaning on the surface of the substrate step by step;
7) setting current parameters of ion cleaning (70A) and anodes (10A-20A), and further carrying out electronic etching on the surface of the substrate step by step;
8) setting process parameters of a planar target, selecting a current mode, wherein the pulse voltage is 1500V, the pulse current is 300A, the average power is 4kW, the pulse width is 100 mus, the frequency is 300Hz, and the duty ratio is 3%;
9) setting the working current of the circular arc target to be 130A, and enabling the electric arc to stably and uniformly contract on the surface of the circular arc target by adjusting the magnetic field;
10) simultaneously starting power supplies of the two technologies to start deposition;
11) and gradually closing the working power supply after 0.5-1 h, and stopping introducing argon gas, namely depositing on the surfaces of Si (100), SUS 304 and the hard alloy to obtain the friction-resistant and corrosion-resistant TiN film.
The SEM surface and cross section of the TiN thin film obtained in this example are shown in FIGS. 2(a) and (d), and the TiN thin film has strong compactness, few pores, no obvious columnar crystal and a deposited film thickness of 1.02 μm.
The resulting TiN film of this example had a coefficient of friction (HiPIMS @ AIP) as shown in FIG. 3, which rose slowly and was significantly better than the comparative TiN film prepared by a single technique.
The wear scar profile of the TiN film obtained in this example is shown in FIG. 4, which shows the best wear scar profile (HiPIMS @ AIP) compared to the comparative TiN film prepared by a single technique.
The friction coefficient and specific wear rate of the TiN thin film obtained in this example are shown in FIG. 5, and the friction coefficient is 0.60, and the specific wear rate (HiPIMS @ AIP) is 5.83X 10-6mm3·(N·m)-1All performed the most excellent.
The anodic polarization curve of the TiN thin film obtained in this example in 3.5 wt.% NaCl aqueous solution is shown in FIG. 6, which (HiPIMS @ AIP) is always in the self-passivation state, and does not show the complete passivation region and the corrosion potential (E)corr) Is-12 mV (SCE), corrosion current density IcorrIs 5.80X 10-8A/cm2。
The surface morphology of the TiN film obtained in this example after the anodizing experiment in 3.5 wt.% NaCl aqueous solution is shown in fig. 7(a), and slight pitting corrosion appears on the surface, which is consistent with the results of the polarization curve data in fig. 6.
Comparative example 1
A method for preparing TiN thin film, using the same substrate, inter-target distance and background vacuum as in example 1, except that:
the resulting TiN film was prepared by deposition for 1h using a single AIP technique.
The SEM surface and cross section of TiN film obtained by the comparative example are shown in figures 2(b) and (e), the compactness is strong, the deposition rate is high, the distribution of large droplets on the surface obviously conforms to the characteristics of the technology, and the thickness of the deposited film is 1.92 mu m.
The friction coefficient of TiN thin film obtained by the present comparative example is shown in FIG. 3, and the friction coefficient (AIP) is superior to that of comparative example 2, which is related to the deposition rate and the plasma density.
The TiN thin film obtained by the present comparative example has a wear scar profile (AIP) as shown in FIG. 4, which is superior to that of comparative example 2 in terms of film hardness, toughness and bonding force.
The friction coefficient and specific wear rate of TiN thin film obtained in this comparative example are shown in FIG. 5, in which the friction coefficient is 0.65 and the specific wear rate (AIP) is 7.5X 10-6mm3·(N·m)-1Consistent with the results of fig. 3 and 4.
The anodic polarization curve of the TiN thin film obtained in the comparative example is shown in figure 6 in a 3.5 wt.% NaCl aqueous solution, and the obvious breakdown-repair characteristics and the breakdown potential (E) of the passivation film appear in the (AIP) passivation regionp) 420mV (SCE), corrosion potential (E)corr) At-59 mV (SCE), corrosion current density (I)corr) Is 4.49X 10-8A/cm2。
The surface morphology of the TiN film obtained in the comparative example after the anodic polarization experiment in the 3.5 wt.% NaCl aqueous solution is shown in figure 7(b), and the surface of the film is partially peeled off, which is consistent with the data result of the polarization curve in figure 6.
Comparative example 2
A method for preparing TiN thin film, using the same substrate, inter-target distance and background vacuum as in example 1, except that:
the resulting TiN film was prepared by deposition for 1h using a single HiPIMS technique.
The SEM surface and cross section of the TiN thin film obtained in the comparative example are shown in FIGS. 2(c) and (f), the surface is uniform, no large-particle droplet defect exists, columnar crystals with a cross section are obvious, the deposition rate is low, and the thickness of the deposited film is 115 nm.
The TiN thin film obtained by the present comparative example has the lowest coefficient of friction (HiPIMS) as shown in FIG. 3.
The profile of the wear scar of the TiN thin film obtained by the comparative example is shown in FIG. 4, and the profile of the wear scar (HiPIMS) shows that the substrate has been worn.
The friction coefficient and specific wear rate of TiN thin film obtained in this comparative example are shown in FIG. 5, and the friction coefficient is 0.77, and the specific wear rate (HiPIMS) is 1.25X 10-5mm3·(N·m)-1Consistent with the results of fig. 3 and 4.
The anodic polarization curve of the TiN thin film obtained in the comparative example in the 3.5 wt.% NaCl aqueous solution is shown in figure 6, and the obvious breakdown-repair characteristic and the breakdown potential (E) of the passivation film appear in the passivation region (HiPIMS)p) 380mV (SCE), corrosion potential (E)corr) At-69 mV (SCE), corrosion current density (I)corr) Is 1.55X 10-7A/cm2。
The surface morphology of the TiN thin film obtained in the comparative example after the anodic polarization experiment in the 3.5 wt.% NaCl aqueous solution is shown in figure 7(c), and the surface of the thin film is partially peeled off, which is consistent with the data result of the polarization curve in figure 6.
The foregoing is only a preferred embodiment of the present invention; the scope of the invention is not limited thereto. Any person skilled in the art should be able to cover the technical scope of the present invention by equivalent or modified solutions and modifications within the technical scope of the present invention.
Claims (5)
1. A preparation method of a friction-resistant and corrosion-resistant TiN film is characterized by comprising the following preparation steps:
1) two opposite plane titanium target materials with the same specification and applied to high-power pulse magnetron sputtering are respectively installed on the inner wall of the equipment deposition cavity, and the distance between the plane titanium target materials and the sample table is adjusted to be 100-300 mm;
2) in the deposition chamber of the equipment, the circular arc target is positioned at the horizontal centers of the two plane targets, the included angle between the circular arc target and the plane targets is 60-120 degrees, and the distance between the circular arc target and the sample table is 100-300 mm;
3) placing the cleaned substrate on a rotating stand, and pumping the deposition chamber to a background vacuum (<8 x 10-3 Pa);
4) introducing argon and nitrogen into the deposition chamber, wherein the flow of the argon is 20-100 sccm, the flow of the nitrogen is 20-100 sccm, the deposition pressure is adjusted to be 0.1-1 Pa, a bias power supply is started, and the sample table autorotates at the speed of 3-10 r/min;
5) the planar target adopts a high-power pulse magnetron sputtering mode, the sputtering voltage is adjusted to be 500-1500V, the sputtering current is adjusted to be 100-400A, the sputtering power is 1-5 kW, the pulse width is 50-500 mus, the frequency is 100-500 Hz, and the duty ratio is 1-10%;
6) the circular arc target adopts an arc ion plating deposition mode, the target working current is set to be 50-200A, and the electric arc can stably and uniformly shrink on the surface of the circular arc target by adjusting the magnetic field.
7) And simultaneously starting a power supply to deposit the TiN film.
2. The method of producing TiN thin film according to the composite deposition technique of claim 1, wherein the purity of the titanium target in the steps 1) and 2) is set to 99.9% or more.
3. The method of producing TiN thin film according to the composite deposition technique of claim 1, wherein the base body of the step 3) is selected from any one of Si substrate, SUS 304 substrate, and cemented carbide substrate.
4. The method of claim 1, wherein the argon purity in step 4) is set to 99.99% or higher.
5. The method for preparing TiN thin film according to the composite deposition technique of claim 1, wherein the sputtering time in the step 7) is 0.5-3 h.
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Citations (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0404973A1 (en) * | 1989-06-27 | 1991-01-02 | Hauzer Holding B.V. | Process and apparatus for coating substrates |
| JP2007307691A (en) * | 2006-05-22 | 2007-11-29 | Mitsubishi Materials Corp | Surface coated cutting tool with hard coated layer exhibiting excellent abrasion resistance in high speed cutting work |
| JP2008006574A (en) * | 2006-06-30 | 2008-01-17 | Mitsubishi Materials Corp | Surface coated cutting tool having hard coated layer exhibiting excellent wear resistance in high speed cutting of heat resistant alloy |
| JP2008173751A (en) * | 2007-01-22 | 2008-07-31 | Mitsubishi Materials Corp | Surface-coated cutting tool provided with hard coated layer achieving excellent wear resistance in high speed cutting |
| US20080260478A1 (en) * | 2005-04-27 | 2008-10-23 | Papken Hovsepian | Pvd Coated Substrate |
| CN103695858A (en) * | 2013-12-26 | 2014-04-02 | 广东工业大学 | Multifunctional fully-automatic ion-plating machine for deposition of cutting tool coating and using method of multifunctional fully-automatic ion-plating machine |
| US20140099489A1 (en) * | 2012-10-04 | 2014-04-10 | Hyundai Motor Company | Coating material for parts of engine exhaust system and method for manufacturing the same |
| CN104862653A (en) * | 2015-05-20 | 2015-08-26 | 魏永强 | Deposition method adopting combination of arc ion plating and high power pulsed magnetron sputtering |
| CN104947046A (en) * | 2015-07-28 | 2015-09-30 | 魏永强 | Multistage magnetic field arc ion plating and high power pulse magnetron sputtering compound deposition method |
| US20160305547A1 (en) * | 2015-04-17 | 2016-10-20 | Mahle Metal Leve S/A | Piston ring for internal combustion engines |
-
2021
- 2021-07-19 CN CN202110812568.3A patent/CN113529038A/en active Pending
Patent Citations (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0404973A1 (en) * | 1989-06-27 | 1991-01-02 | Hauzer Holding B.V. | Process and apparatus for coating substrates |
| US20080260478A1 (en) * | 2005-04-27 | 2008-10-23 | Papken Hovsepian | Pvd Coated Substrate |
| JP2007307691A (en) * | 2006-05-22 | 2007-11-29 | Mitsubishi Materials Corp | Surface coated cutting tool with hard coated layer exhibiting excellent abrasion resistance in high speed cutting work |
| JP2008006574A (en) * | 2006-06-30 | 2008-01-17 | Mitsubishi Materials Corp | Surface coated cutting tool having hard coated layer exhibiting excellent wear resistance in high speed cutting of heat resistant alloy |
| JP2008173751A (en) * | 2007-01-22 | 2008-07-31 | Mitsubishi Materials Corp | Surface-coated cutting tool provided with hard coated layer achieving excellent wear resistance in high speed cutting |
| US20140099489A1 (en) * | 2012-10-04 | 2014-04-10 | Hyundai Motor Company | Coating material for parts of engine exhaust system and method for manufacturing the same |
| CN103695858A (en) * | 2013-12-26 | 2014-04-02 | 广东工业大学 | Multifunctional fully-automatic ion-plating machine for deposition of cutting tool coating and using method of multifunctional fully-automatic ion-plating machine |
| US20160305547A1 (en) * | 2015-04-17 | 2016-10-20 | Mahle Metal Leve S/A | Piston ring for internal combustion engines |
| CN104862653A (en) * | 2015-05-20 | 2015-08-26 | 魏永强 | Deposition method adopting combination of arc ion plating and high power pulsed magnetron sputtering |
| CN104947046A (en) * | 2015-07-28 | 2015-09-30 | 魏永强 | Multistage magnetic field arc ion plating and high power pulse magnetron sputtering compound deposition method |
Non-Patent Citations (3)
| Title |
|---|
| J. VETTER 等: "Characterization of advanced coating architectures deposited by an arc-HiPIMS hybrid process", 《SURFACE AND COATINGS TECHNOLOGY》 * |
| W.D. MUNZ 等: "A new concept for physical vapor deposition coating combing the methods of arc evaporation and unbalanced-magnetron sputtering", 《SURFACE AND COATINGS TECHNOLOY》 * |
| 张权 等: "先进复合物理气相沉积技术制备高性能硬质涂层", 《工具技术》 * |
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Application publication date: 20211022 |