CN106119784B - A kind of Ti-Al-Mo-N multicomponent hards Gradient Film and its preparation method and application - Google Patents

Abstract

The invention relates to a Ti-Al-Mo-N multi-component hard gradient film and its preparation method and application; it belongs to the technical field of special material preparation. The Ti-Al-Mo-N multi-component hard gradient film of the present invention includes the following components in terms of mass percentage: Ti 55%-85%, Al 8%-30%, Mo 4%-15%, N 3% -25%. The gradient film is prepared by arc ion plating to form a coating with matrix/TiN/Ti-Al-Mo-N; the coating can be used in the fields of papermaking and printing. The invention has reasonable component design, simple process, and is convenient for large-scale application, especially large-scale application in the printing field.

Description

A kind of Ti-Al-Mo-N multi-component hard gradient film and its preparation method and application

technical field

The invention relates to a Ti-Al-Mo-N multi-component hard gradient film and a preparation method and application thereof; it belongs to the technical field of preparation of special materials.

Background technique

Arc ion plating is to trigger the ignition arc between the cathode and the anode. The arc discharge is only carried out at one or several dense arc spots on the surface of the target. The whole moving target is consumed evenly. In cathodic arc deposition, the deposition material is evaporated by the action of vacuum arc. In the arc line, the source material is used as the cathode. Most of the basic processes of the arc occur at the arc point in the cathode area. The typical size of a few micrometers, and have a very high current density. The evaporated product obtained by arc evaporation consists of electrons, ions, neutral gas phase atoms and particles. The plasma is directly generated from the cathode without a molten pool, and the cathode target can be arranged in any direction according to the shape of the workpiece, which greatly simplifies the fixture.

Arc ion plating has developed rapidly because of its high deposition rate, simple cleaning process for workpieces before coating, and no impact on the environment. Under vacuum conditions, gas glow discharge is used to ionize the gas to produce an ion bombardment effect, and finally the evaporant and reactant are deposited on the substrate. Products deposited by arc ion plating generally have strong film adhesion, and the continuous bombardment of high-energy particles can promote the surface diffusion and chemical metallurgical combination of the film layer; compared with electroless plating, electroplating, and thermal spraying, the film layer of arc ion plating products is uniform Good performance, high film density, fast film deposition rate, and good heating uniformity.

Arc ion plating TiN product hardness can generally reach about 2000HV, and with the innovation of technology, TiN was often compared with Al ₂ O ₃ as early as the rise of TiN. When arc ion plating TiN introduces Al elements to form TiAlN products, due to the addition of Al and the diffusion of Al to the surface at high temperature, a layer of aluminum oxide protective film will be formed, which is very helpful for the wear resistance and corrosion resistance of the coating.

At present, the main research points of using arc ion plating technology to prepare multi-component film layers are: 1. The combined use and composition of alloy targets and pure metal targets. 2. The bonding force between the film base and the bonding force between the film layers. 3. Maximize hardness. But so far, there is no report at home and abroad on the preparation of wear-resistant and corrosion-resistant Ti-Al-Mo-N multi-component hard gradient coating materials by arc ion plating on the surface of the substrate such as SKD2 ink scraper.

Contents of the invention

Aiming at the defects of the prior art, the invention provides a Ti-Al-Mo-N multi-component hard gradient film and its preparation method and application.

A Ti-Al-Mo-N multi-component hard gradient film of the present invention; comprises the following components in terms of mass percentage:

Ti 55%-85%, preferably 67%-83%, more preferably 70%-80%;

Al 8%-30%, preferably 10%-21%, more preferably 12%-20%;

Mo 4%-15%, preferably 4%-12%, more preferably 5%-10%;

N 3%-25%, preferably 3%-23%, more preferably 3%-22%.

A method for preparing a Ti-Al-Mo-N multi-component hard gradient film of the present invention includes the following scheme: using a Ti-Al-Mo alloy target as a raw material, and preparing a Ti-Al-Mo alloy target on the surface of a workpiece by arc ion plating Al-Mo-N multi-component hard gradient film; before arc ion plating, control the vacuum in the deposition furnace to be less than or equal to 0.03Pa; The current of the Mo alloy target is 70-80A, the rotational speed of the workpiece is controlled at 4-6r/min, and the plating temperature is controlled at 450-500°C;

The Ti-Al-Mo alloy target includes the following components in mass percentage:

Ti 55%-85%;

Al 10%-30%;

Mo 5%-15%.

The invention relates to a method for preparing a Ti-Al-Mo-N multi-component hard gradient film. During arc ion plating, the deposition time is controlled to be 20-30 minutes.

A method for preparing a Ti-Al-Mo-N multi-component hard gradient film of the present invention, the method for preparing the Ti-Al-Mo alloy target is as follows:

Pure titanium, pure aluminum, and Ti-Mo master alloy are selected according to the designed composition as raw materials, and vacuum smelting is carried out at least 2 times, preferably 3 times, on the prepared raw materials to obtain the Ti-Al-Mo alloy target.

The pure titanium is industrial pure titanium with a purity greater than or equal to 99.9%; the pure aluminum is industrial high-purity Al with a purity greater than or equal to 99.9%; the mass percentage of impurities in the Ti-Mo master alloy is less than 0.1% .

The application of a Ti-Al-Mo-N multi-component hard gradient film of the present invention includes using the Ti-Al-Mo-N multi-component hard gradient film as a coating, and the structure of the coating is It is matrix/TiN/Ti-Al-Mo-N.

Preferably, in the application of a Ti-Al-Mo-N multi-component hard gradient film of the present invention, the thickness of TiN in the coating is 0.5-1.2 microns. The mass percent content of N in the TiN is 16-25%, and the balance is Ti.

Preferably, in the application of a Ti-Al-Mo-N multi-component hard gradient film of the present invention, the thickness of Ti-Al-Mo-N in the coating is 1.5-3.0 microns.

As a preference, the application of a Ti-Al-Mo-N multi-component hard gradient film of the present invention, the substrate is selected from SKD1 ink scraper, SKD2 ink scraper, ROE ink scraper, ABE ink scraper, SKH-2 ink scraper At least one of them, preferably SKD2 ink scraper.

As preferably, the application of a Ti-Al-Mo-N multi-component hard gradient film of the present invention, the preparation method of the coating comprises the following steps:

step one

Place a substrate with a clean surface and a surface roughness Ra of 0.07-0.09um, preferably 0.08um, in the arc ion plating equipment, vacuumize until the pressure in the arc ion plating equipment is 0.03-0.003Pa, and then pass argon gas to When the pressure in the arc ion plating equipment is 0.16-0.22Pa, turn on the low-energy ion source, control the temperature in the arc ion plating equipment to 200°C-250°C, control the accelerating voltage to 2.3-6.0Kv, preferably 4.0Kv, and the arc current 80-100A, activate and clean the base material; obtain the activated base material;

step two

Use pure Ti as the Ti target, place the Ti target and the activated substrate obtained in step 1 in the arc ion plating equipment, vacuumize until the pressure in the arc ion plating equipment is 0.03-0.003Pa, and control the bias voltage of the activated substrate as -400～-450V; then pass N gas into the arc ion plating equipment, the partial pressure of N gas is 1.2-1.4Pa (because there is only one reaction gas in the reaction membrane chamber, the partial pressure of N gas is the total pressure. ) and control the current of the Ti target to be 55-60A, perform arc ion plating, and finally turn off the control power supply, and cool down to room temperature with the arc ion plating equipment to obtain a substrate with a TiN layer; when performing arc ion plating, control the activated base The rotation speed of the material is 4~6r/min, and the control plating temperature is 380-400℃;

step three

Place the substrate with TiN layer and Ti-Al-Mo alloy target obtained in step 2 in the arc ion plating equipment, vacuumize until the pressure in the arc ion plating equipment is 0.03-0.003Pa, and control the bias voltage of the activated substrate at the same time It is -400～-450V, the partial pressure of N gas that is fed into the arc ion plating equipment is 2.2-2.66Pa, and the current of the Ti-Al-Mo alloy target is controlled to 70-80A, and the arc ion plating is performed. The coating is obtained; when arc ion plating is performed, the rotation speed of the base material with the TiN layer is controlled to be 4-6 r/min, and the plating temperature is controlled to be 450-500° C.

As a preferred solution, in step 1, the substrate is activated and cleaned for 10-15 minutes.

In industrial applications, substrates with a clean surface and a surface roughness Ra of 0.07-0.09um are prepared by the following scheme:

The substrate (such as SKD2 ink scraper substrate) is mechanically polished on a polishing machine to about Ra0.08um. The polished samples were washed with clean water, dried and placed in the sample pan. Use absorbent cotton dipped in acetone to wipe the plating surface to remove surface oil, rust, oxide layer and impurities. After wiping with acetone, rinse with clean water, and put it into a beaker containing alcohol for ultrasonic cleaning for 10-15min. After the ultrasound is completed, take out the deionized water to clean, dry, and wait for plating.

As a preferred solution, in step 2, the time for arc ion plating is 15-20min.

As a preferred solution, in step 3, the time for arc ion plating is 20-30 minutes.

As a preferred solution, in step 3, after the arc ion plating is completed, the control power supply is turned off, and the arc ion plating equipment is cooled to room temperature.

As a preferred solution, the arc ion plating equipment is a Bulat-6 multi-arc ion coating machine. The coating machine is composed of vacuum system, coating system, and electrical control system, without additional magnetic filtration system. There are three arc sources in the coating chamber, and the arc sources on the left and right sides are used to initiate arc deposition.

When the arc ion plating equipment is a Bulat-6 multi-arc ion coating machine, the Ti target is a circular target; the diameter of the circular target is φ60 mm, and the thickness is 42 mm.

When the arc ion plating equipment is a Bulat-6 multi-arc ion coating machine, after the arc ion plating in step 3 is completed, the Hall control power supply is turned off, and the workpiece is taken out with the membrane chamber cooled to room temperature, sealed and stored for testing. After the workpiece is taken out, the ion coating machine needs to be vacuumed for the next use.

The targets involved in the present invention, such as Ti targets and Ti-Al-Mo alloy targets, can be processed according to the actual required size.

The coating designed by the invention can be used in papermaking, printing and other fields.

Principle advantage

The present invention uses the arc ion plating technology to pretreat the substrate (such as the surface of an ink scraper) by Ar gas bombardment; then feeds N gas to deposit a TiN coating to improve the bonding force between the multi-component hard coatings; A good self-made alloy target is deposited on the workpiece to obtain a hard coating with excellent wear resistance and corrosion resistance.

The present invention adopts the arc ion plating technology, and through the synergy of substrate pretreatment process system, workpiece bias voltage during plating, nitrogen partial pressure, plating time, arc current, workpiece speed and other parameters, the obtained coating has achieved unexpected results. Effect, especially to achieve a good match between the mechanical properties and performance of the coating.

Principles and advantages

At the same time, the present invention also aims at the defects in the performance of domestic scraper products, and provides a coating with a matrix/TiN/Ti-Al-Mo-N structure by adding Mo element into the stable binary system hard film TiAlN . When the coating is used for printing and papermaking, it has unexpected effects, and the possible reasons are:

Mo has solid self-lubricating properties, and it can form MoO3 phase in the process of friction and wear, which has good wear resistance and friction reduction effect. This system can not only exert the corrosion resistance function of Al element to form the aluminum oxide protective film, but also exert the excellent wear resistance and friction reduction of Mo element, thereby greatly improving its use effect.

The coating structure of the present invention is substrate/TiN/Ti-Al-Mo-N. A layer of TiN is plated on the substrate first for better adhesion between the film layers, and Mo is added to the mature Ti-Al system. Elements significantly enhance the wear resistance of the coating.

Compared with methods such as laser cladding and thermal spraying, the method of the present invention can deposit at a lower temperature (generally around 500° C.), which can avoid the influence of mechanical properties caused by thermal inhomogeneity; compared to chemical vapor phase For methods such as deposition and electroless plating, the method of the present invention has simple production methods, high ionization rate, large production benefits, and is more conducive to realizing market industrialization. Arc ion plating Ti-Al-Mo-N not only broadens the field of material production, reduces production costs, improves production efficiency, but also effectively improves the corrosion resistance and wear resistance of the coating.

In a word, the present invention achieves excellent results through the design of the components of the multi-component hard gradient membrane and the synergy of the preparation parameters of the component hard gradient membrane. At the same time, when the multi-component hard gradient membrane design structure is applied When coating, the coating has shown unexpected advantages in papermaking, printing and other fields.

Detailed ways

Aiming at the current problems of fast wear and low efficiency of ink scrapers, the invention provides a preparation method of a wear-resistant and corrosion-resistant hard coating.

Example 1

(1) Determination of deposition technology and preparation of alloy targets:

The Bulat-6 multi-arc ion coating machine is used to deposit the coating. The coating machine is composed of a vacuum system, a coating system, and an electrical control system without an additional magnetic filter system. There are three arc sources in the coating chamber, and the arc sources on the left and right sides are used to initiate arc deposition.

The design, selection and preparation of the target material: when TIN coating is applied, the commercially pure titanium target purchased is selected, the purity is 99.9%, and the shape of the titanium target is processed into a circular target with a diameter of φ60mm and a thickness of 42mm according to the requirements of the equipment. When the Ti-Al-Mo-N coating is applied, the target material is a self-made alloy target. The composition of the alloy target is designed as follows: the mass percentage of Ti is 75%, the mass percentage of Al is 20%, and the mass percentage of Mo is 5%. The alloy targets are all vacuum smelted three times through a vacuum induction melting furnace. The smelted alloy materials are: industrial pure titanium with a purity of 99.9%; industrial high-purity Al with a purity of 99.9%; Ti-Mo master alloy with a purity of 99.9%.

The prepared target is processed into the required size by wire cutting technology according to the requirements of the equipment.

(2) Substrate pretreatment:

① Chemical decontamination treatment: Mechanically polish the ink scraper substrate on a polishing machine to about Ra0.08um. The polished samples were washed with clean water, dried and placed in the sample pan. Use absorbent cotton dipped in acetone to wipe the plating surface to remove surface oil, rust, oxide layer and impurities. After wiping with acetone, rinse with water, put it into a beaker with alcohol and ultrasonically clean it for 15 minutes. After the ultrasound is completed, take out the deionized water to clean, dry, and wait for plating.

②Ar gas pretreatment process: Before ion coating, the vacuum background of the membrane chamber is pumped to 0.03Pa and Ar gas is introduced. The voltage is 4.0Kv, the arc current is 80A, and the sample is activated and cleaned for 15 minutes.

(3) Arc ion plating deposition coating process:

① The plating process of the TiN film layer is determined: the film chamber is vacuumed to 0.03Pa, the substrate is biased at -420V, N gas is introduced, and the N gas pressure is kept at 1.25Pa. The titanium target arc current is adjusted to 58A, and the workpiece speed is maintained at 5r/ min, the plating temperature is 400°C, and the deposition time is 15 min.

②The plating process of Ti-Al-Mo-N film layer is determined: according to the requirements of the coating structure, the substrate is plated with TiN. Turn off the Hall control power supply, cool the TiN workpiece to room temperature with the film cavity after plating, calibrate the vacuum to 0.03Pa, apply a -450V bias voltage to the substrate, and keep the N pressure at 2.66Pa, and adjust the alloy target arc current to 73A. The rotational speed was kept at 5r/min, the plating temperature was 470°C, and the deposition time was 30min.

③ After the deposition is completed, turn off the Hall control power supply, and the workpiece is taken out with the membrane cavity cooled to room temperature, and sealed and stored for testing. After taking it out, the ion coating machine needs to be vacuumed for the next use. In the obtained Ti-Al-Mo-N film layer, by mass percent, it is composed of the following components:

Ti 71%, Al 18%, Mo 4%, N 7%.

According to the SEM test, the thickness of TiN+Ti-Al-Mo-N is about 3.4um; the hardness HIT measured by the nanohardness tester is 3.54GPa, and the elastic modulus EIT of the coating is 400.6Gpa; after the electrochemical experiment test, The corrosion current density of the coating is 3.29uA, compared with the substrate corrosion current density of 19.3uA, and the corrosion resistance after plating is improved by about 6 times.

Example 2

(1) Determination of deposition technology and preparation of alloy targets:

The Bulat-6 multi-arc ion coating machine is used to deposit the coating. The coating machine is composed of a vacuum system, a coating system, and an electrical control system without an additional magnetic filter system. There are three arc sources in the coating chamber, and the arc sources on the left and right sides are used to initiate arc deposition.

The design, selection and preparation of the target material: when TIN coating is applied, the commercially pure titanium target purchased is selected, the purity is 99.9%, and the shape of the titanium target is processed into a circular target with a diameter of φ60mm and a thickness of 42mm according to the requirements of the equipment. When the Ti-Al-Mo-N coating is applied, the target material is a self-made alloy target. The composition of the alloy target is designed as follows: the mass percentage of Ti is 75%, the mass percentage of Al is 18%, and the mass percentage of Mo is 7%. The alloy targets are all vacuum smelted three times through a vacuum induction melting furnace. The smelted alloy materials are: industrial pure titanium with a purity of 99.9%; industrial high-purity Al with a purity of 99.9%; Ti-Mo master alloy with a purity of 99.9%.

The prepared target is processed into the required size by wire cutting technology according to the requirements of the equipment.

(2) Substrate pretreatment:

① Chemical decontamination treatment: Mechanically polish the SKD2 ink scraper substrate on a polishing machine to about Ra0.08um. The polished samples were washed with clean water, dried and placed in the sample pan. Use absorbent cotton dipped in acetone to wipe the plating surface to remove surface oil, rust, oxide layer and impurities. After wiping with acetone, rinse with water, put it into a beaker with alcohol and ultrasonically clean it for 15 minutes. After the ultrasound is completed, take out the deionized water to clean, dry, and wait for plating.

②Ar gas pretreatment process: Before ion coating, the vacuum background of the membrane chamber is pumped to 0.03Pa and Ar gas is introduced. The voltage is 4.0Kv, the arc current is 100A, and the sample is activated and cleaned for 15 minutes.

(3) Arc ion plating deposition coating process:

① The plating process of the TiN film layer is determined: the film chamber is vacuumed to 0.03Pa, the substrate is biased at -450V, N gas is introduced, and the N gas pressure is kept at 1.35Pa. The titanium target arc current is adjusted to 60A, and the workpiece speed is maintained at 5r/ min, the plating temperature is 400°C, and the deposition time is 10 min.

②The plating process of Ti-Al-Mo-N film layer is determined: according to the requirements of the coating structure, the substrate is plated with TiN. Turn off the Hall control power supply, cool the TiN workpiece to room temperature with the film cavity after plating, calibrate the vacuum to 0.03Pa, apply -450V bias voltage to the substrate, and keep the N pressure at 2.45Pa, and adjust the alloy target arc current to 80A. The rotational speed was kept at 5r/min, the plating temperature was 500°C, and the deposition time was 20min.

③ After the deposition is completed, turn off the Hall control power supply, and the workpiece is taken out with the membrane cavity cooled to room temperature, and sealed and stored for testing. After taking it out, the ion coating machine needs to be vacuumed for the next use. In the obtained Ti-Al-Mo-N film layer, by mass percent, it is composed of the following components:

Ti 70%, Al 15%, Mo 6%, N 9%.

According to the SEM test, the thickness of TiN+Ti-Al-Mo-N is about 2.34um; the hardness HIT measured by the nanohardness tester is 3.96GPa, and the elastic modulus EIT of the coating is 344.6Gpa; through the electrochemical experiment test, The corrosion current density of the coating is 3.35uA, compared with the substrate corrosion current density of 19.3uA, and the corrosion resistance after plating is improved by about 6 times.

Example 3

(1) Determination of deposition technology and preparation of alloy targets:

The Bulat-6 multi-arc ion coating machine is used to deposit the coating. The coating machine is composed of a vacuum system, a coating system, and an electrical control system without an additional magnetic filter system. There are three arc sources in the coating chamber, and the arc sources on the left and right sides are used to initiate arc deposition.

The design, selection and preparation of the target material: when TIN coating is applied, the commercially pure titanium target purchased is selected, the purity is 99.9%, and the shape of the titanium target is processed into a circular target with a diameter of φ60mm and a thickness of 42mm according to the requirements of the equipment. When the Ti-Al-Mo-N coating is applied, the target material is a self-made alloy target. The composition of the alloy target is designed as follows: the mass percentage of Ti is 70%, the mass percentage of Al is 15%, and the mass percentage of Mo is 15%. The alloy targets are all vacuum smelted three times through a vacuum induction melting furnace. The smelted alloy materials are: industrial pure titanium with a purity of 99.9%; industrial high-purity Al with a purity of 99.9%; Ti-Mo master alloy with a purity of 99.9%.

The prepared target is processed into the required size by wire cutting technology according to the requirements of the equipment.

(2) Substrate pretreatment:

① Chemical decontamination treatment: Mechanically polish the ink scraper substrate on a polishing machine to about Ra0.08um. The polished samples were washed with clean water, dried and placed in the sample pan. Use absorbent cotton dipped in acetone to wipe the plating surface to remove surface oil, rust, oxide layer and impurities. After wiping with acetone, rinse with water, put it into a beaker with alcohol and ultrasonically clean it for 15 minutes. After the ultrasound is completed, take out the deionized water to clean, dry, and wait for plating.

②Ar gas pretreatment process: Before ion coating, the vacuum background of the membrane chamber is pumped to 0.03Pa and Ar gas is introduced. When the furnace pressure rises to 0.20Pa, the low-energy ion source is turned on. The voltage is 4.0Kv, the arc current is 85A, and the sample is activated and cleaned for 15 minutes.

(3) Arc ion plating deposition coating process:

① The plating process of the TiN film layer is determined: the film chamber is vacuumed to 0.03Pa, the substrate is biased at -400V, N gas is introduced, and the N gas pressure is kept at 1.30Pa. The titanium target arc current is adjusted to 55A, and the workpiece speed is maintained at 5r/ min, the plating temperature is 400°C, and the deposition time is 15 min.

②The plating process of Ti-Al-Mo-N film layer is determined: according to the requirements of the coating structure, the substrate is plated with TiN. Turn off the Hall control power supply, cool the TiN workpiece to room temperature with the film cavity after plating, calibrate the vacuum to 0.03Pa, apply a -450V bias voltage to the substrate, and keep the N pressure at 2.50Pa, and adjust the alloy target arc current to 75A. The rotational speed was maintained at 5r/min, the plating temperature was 450°C, and the deposition time was 30min.

③ After the deposition is completed, turn off the Hall control power supply, and the workpiece is taken out with the membrane cavity cooled to room temperature, and sealed and stored for testing. After taking it out, the ion coating machine needs to be vacuumed for the next use. In the obtained Ti-Al-Mo-N film layer, by mass percent, it is composed of the following components:

Ti 65%, Al 10%, Mo 10%, N 15%.

According to the SEM test, the thickness of TiN+Ti-Al-Mo-N is about 4.13um; the hardness HIT measured by the nanohardness tester is 2.97GPa, and the elastic modulus EIT of the coating is 344.9Gpa; the electrochemical experiment test shows that The corrosion current density of the coating is 3.82uA, compared with the substrate corrosion current density of 19.3uA, and the corrosion resistance after plating is improved by about 5 times.

Example 4

(1) Determination of deposition technology and preparation of alloy targets:

The Bulat-6 multi-arc ion coating machine is used to deposit the coating. The coating machine is composed of a vacuum system, a coating system, and an electrical control system without an additional magnetic filter system. There are three arc sources in the coating chamber, and the arc sources on the left and right sides are used to initiate arc deposition.

The design, selection and preparation of the target material: when TIN coating is applied, the commercially pure titanium target purchased is selected, the purity is 99.9%, and the shape of the titanium target is processed into a circular target with a diameter of φ60mm and a thickness of 42mm according to the requirements of the equipment. When the Ti-Al-Mo-N coating is applied, the target material is a self-made alloy target. The composition of the alloy target is designed as follows: the mass percentage of Ti is 80%, the mass percentage of Al is 15%, and the mass percentage of Mo is 5%. The alloy targets are all vacuum smelted three times through a vacuum induction melting furnace. The smelted alloy materials are: industrial pure titanium with a purity of 99.9%; industrial high-purity Al with a purity of 99.9%; Ti-Mo master alloy with a purity of 99.9%.

The prepared target is processed into the required size by wire cutting technology according to the requirements of the equipment.

(2) Substrate pretreatment:

① Chemical decontamination treatment: Mechanically polish the ink scraper substrate on a polishing machine to about Ra0.08um. The polished samples were washed with clean water, dried and placed in the sample pan. Use absorbent cotton dipped in acetone to wipe the plating surface to remove surface oil, rust, oxide layer and impurities. After wiping with acetone, rinse with water, put it into a beaker with alcohol and ultrasonically clean it for 15 minutes. After the ultrasound is completed, take out the deionized water to clean, dry, and wait for plating.

②Ar gas pretreatment process: Before ion coating, the vacuum background of the membrane chamber is pumped to 0.03Pa and Ar gas is introduced. The voltage is 4.0Kv, the arc current is 100A, and the sample is activated and cleaned for 15 minutes.

(3) Arc ion plating deposition coating process:

① The plating process of the TiN film layer is determined: the film chamber is vacuumed to 0.03Pa, the substrate is biased at -450V, N gas is introduced, and the N gas pressure is kept at 1.40Pa. The titanium target arc current is adjusted to 60A, and the workpiece speed is maintained at 5r/ min, the plating temperature is 400°C, and the deposition time is 20min.

②The plating process of Ti-Al-Mo-N film layer is determined: according to the requirements of the coating structure, the substrate is plated with TiN. Turn off the Hall control power supply, cool the TiN workpiece to room temperature with the film cavity after plating, calibrate the vacuum to 0.03Pa, apply -450V bias voltage to the substrate, and keep the N pressure at 2.66Pa, and adjust the alloy target arc current to 80A. The rotational speed was kept at 5r/min, the plating temperature was 500°C, and the deposition time was 30min.

③ After the deposition is completed, turn off the Hall control power supply, and the workpiece is taken out with the membrane cavity cooled to room temperature, and sealed and stored for testing. After taking it out, the ion coating machine needs to be vacuumed for the next use. In the obtained Ti-Al-Mo-N film layer, by mass percent, it is composed of the following components:

Ti 72%, Al 10%, Mo 4%, N 14%.

According to the SEM test, the thickness of TiN+Ti-Al-Mo-N is about 4.79um; the hardness HIT measured by the nanohardness tester is 4.16GPa, and the elastic modulus EIT of the coating is 375.3Gpa; the electrochemical experiment test shows that The corrosion current density of the coating is 2.78uA, compared with the substrate corrosion current density of 19.3uA, and the corrosion resistance after plating is improved by about 7 times.

The beneficial effects brought by the technical solutions provided by the embodiments of the present invention are: compared with the optimum hardness value of 1200HV of the Ni-P-Cu-TiN coating prepared by electric brush plating, the hardness of the coating by the method of the present invention is greatly increased, Moreover, the deposited film layer is uniform, the film layer density is high, and the time is greatly shortened.

Claims (5)

1. an application of a Ti-Al-Mo-N multi-component hard gradient film, characterized in that: comprising using the Ti-Al-Mo-N multi-component hard gradient film as a coating, the The structure of the coating is matrix/TiN/Ti-Al-Mo-N; The Ti-Al-Mo-N multi-component hard gradient film includes the following components in mass percent: Ti 55%-85%; Al 8%-30%; Mo 4%-15%; N 3%-25%; The preparation method of described coating comprises the steps: step one Put the substrate with a clean surface and a surface finish Ra of 0.07-0.09um in the arc ion plating equipment, vacuumize until the pressure in the arc ion plating equipment is 0.03-0.003Pa, and then pass argon gas into the arc ion plating equipment When the pressure is 0.16-0.22Pa, turn on the low-energy ion source, control the temperature in the arc ion plating equipment to 200°C-250°C, control the accelerating voltage to 2.3-6.0kV, and the arc current to 80-100A to activate the substrate cleaning; obtaining activated substrate; step two Using pure Ti as the Ti target, place the Ti target and the activated substrate obtained in step 1 in the arc ion plating equipment, vacuumize until the pressure in the arc ion plating equipment is 0.03-0.003Pa, and control the bias voltage of the activated substrate to be -400～-450V; then feed N gas to the partial pressure of N gas in the arc ion plating equipment to 1.2-1.4Pa; and control the current of the Ti target to 55-60A for arc ion plating, and finally turn off the control power , with the arc ion plating equipment cooled to room temperature, a substrate with a TiN layer is obtained; when performing arc ion plating, the rotation speed of the activated substrate is controlled to be 4-6r/min, and the plating temperature is controlled to be 380-400°C; step three Place the substrate with TiN layer and Ti-Al-Mo alloy target obtained in step 2 in the arc ion plating equipment, vacuumize until the pressure in the arc ion plating equipment is 0.03-0.003Pa, and control the bias voltage of the activated substrate at the same time It is -400～-450V, the partial pressure of N gas that is fed into the arc ion plating equipment is 2.2-2.66Pa, and the current of the Ti-Al-Mo alloy target is controlled to 70-80A, and the arc ion plating is carried out. The coating is obtained; when arc ion plating is performed, the rotation speed of the base material with the TiN layer is controlled to be 4-6 r/min, and the plating temperature is controlled to be 450-500° C. 2. the application of a kind of Ti-Al-Mo-N multicomponent hard gradient film according to claim 1, is characterized in that: The thickness of TiN in the coating is 0.5-1.2 microns, the mass percentage of N in the TiN is 16-25%, and the balance is Ti; The thickness of Ti-Al-Mo-N in the coating is 1.5-3.0 microns. 3. the application of a kind of Ti-Al-Mo-N multicomponent hard gradient film according to claim 1, is characterized in that: The substrate is selected from at least one of SKD1 ink scraper, SKD2 ink scraper, ROE ink scraper, ABE ink scraper, and SKH-2 ink scraper. 4. the application of a kind of Ti-Al-Mo-N multi-component hard gradient film according to claim 1, is characterized in that: In step 1, the substrate is activated and cleaned for 10-15 minutes; In step 2, the time for arc ion plating is 15-20min; In step 3, the time for arc ion plating is 20-30 minutes. 5. the application of a kind of Ti-Al-Mo-N multi-component hard gradient film according to claim 1, is characterized in that; The preparation method of described Ti-Al-Mo alloy target is: Allocation of pure titanium, pure aluminum, and Ti-Mo master alloy as raw materials according to the designed composition, and performing vacuum smelting on the prepared raw materials at least twice to obtain the Ti-Al-Mo alloy target.