CN114921759B - Multi-arc ion plating coating process - Google Patents
Multi-arc ion plating coating process Download PDFInfo
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- CN114921759B CN114921759B CN202210539640.4A CN202210539640A CN114921759B CN 114921759 B CN114921759 B CN 114921759B CN 202210539640 A CN202210539640 A CN 202210539640A CN 114921759 B CN114921759 B CN 114921759B
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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
- C23C14/24—Vacuum evaporation
- C23C14/32—Vacuum evaporation by explosion; by evaporation and subsequent ionisation of the vapours, e.g. ion-plating
- C23C14/325—Electric arc evaporation
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22C—FOUNDRY MOULDING
- B22C9/00—Moulds or cores; Moulding processes
- B22C9/22—Moulds for peculiarly-shaped castings
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C12/00—Alloys based on antimony or bismuth
-
- 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
-
- 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
- C23C14/02—Pretreatment of the material to be coated
- C23C14/021—Cleaning or etching treatments
- C23C14/022—Cleaning or etching treatments by means of bombardment with energetic particles or radiation
-
- 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
- C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
- C23C14/0664—Carbonitrides
-
- 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
- C23C14/54—Controlling or regulating the coating process
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Mechanical Engineering (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Physical Vapour Deposition (AREA)
Abstract
The invention discloses a multi-arc ion plating coating process. The process comprises the following steps: step 1, preprocessing a base material; step 2, plating a TiN transitional coating on the magnetic control multi-arc ion plating; step 3, magnetically controlling the multi-arc ion plating TiTaN coating; and 4, magnetically controlling the multi-arc ion plating TiTaN-BiScCoCN coating. The substrate is etched by adopting glow discharge and ion bombardment, so that the bonding strength of the coating and the substrate is improved, meanwhile, the substrate is subjected to multi-arc ion plating TiTaN-BiScCoCN coating by using a magnetic control arc technology, a TaTi target is adopted as a target for secondary coating, and a Co target and a BiScC target are adopted in tertiary coating, so that the coating is better in bonding, and the compactness and wear resistance of the coating are improved. Compared with the prior art, the TiTaN-BiScCoCN coating prepared by the multi-arc ion plating coating process has the advantages of good wear resistance, good hot salt corrosion resistance and good bonding strength with a base material.
Description
Technical Field
The invention relates to the technical field of surface protection coatings, in particular to a multi-arc ion plating coating process.
Background
The material surface technology can be roughly classified into surface coating technology, surface modification technology and thin film technology. The specific process comprises the following steps: electroplating, coating, overlaying, thermal spraying, thermal diffusion, chemical conversion, vapor deposition, three-beam modification and the like. Film forming technologies in thin film technology are classified into two types, namely: physical vapor deposition technology and chemical vapor deposition technology, namely, atoms of one or more special materials are transferred to the surface of another material through a complex physical or chemical method, so that the material with special functions is combined with the surface material of an object to be optimized, and the surface of the object to be optimized obtains special properties, such as higher hardness, lower friction coefficient, smaller surface roughness and the like. Chemical vapor deposition, namely, by utilizing a chemical principle, a material with special performance is gasified to participate in a specific chemical reaction, solid matters generated by the reaction are deposited on the surface of a substrate, and finally, a film layer with special performance is formed on the surface of the substrate, but the deposition temperature is higher, so that the reaction gas and a device are easy to generate chemical reaction to generate impurities, and the film manufacturing cost is increased. The metallographic structure of the surface of the matrix is easy to change at high temperature, and the purity and stability of the film are affected. Physical vapor deposition techniques can be broadly divided into three types, vacuum evaporation, sputter plating, and ion plating. VacuumThe evaporation plating is to evaporate or vaporize the solid target material in a high temperature state by using heating methods such as resistance, laser or induction heating, and then deposit the solid target material on the surface of the substrate to form a film layer, but the uniformity of the deposited film is poor and the bonding force between the deposited film and the substrate is low; the sputtering plating utilizes high-energy inert gas ions to impact the surface of the target under the action of an electric field, a magnetic field or a composite field, and in the high-energy collision process, energy transmission and loss occur to generate a large amount of target ions or ion clusters separated from the surface of the target and a large amount of heat,however, the method is thatThen, under the action of a specific physical transmission field, the film is deposited on the surface of the substrate to form a film, but the working air pressure is higher, and the deposition speed is too slow, so that the practical application of the traditional sputtering film is limited; ion plating is to deposit ions on the surface of a target material to the surface of a substrate under the action of a strong electric field according to the principles of glow discharge or arc discharge and the like to form a film, wherein the multi-arc ion plating technology in arc ion plating has become one of the mainstream technologies in the current industrial production.
The multi-arc ion plating combines the characteristics of vacuum evaporation plating and sputtering plating, a plating material is used as a target cathode, a plasma region is formed by utilizing vacuum arc discharge, target particles evaporated by the arc discharge are ionized after moving to the plasma region, and charged target particles are accelerated to move to the surface of a substrate under the drive of negative bias and then deposited to form a film. The most remarkable characteristic of multi-arc ion plating is that a molten pool is not needed, plasma can be directly generated from a cathode, a cathode target can be freely distributed according to the shape of a workpiece, and the multi-arc ion plating equipment is greatly simplified. Meanwhile, the ionization excited particles have high energy, so that the prepared film has high density, good strength and durability and good bonding strength between film layers. However, the problems of instability of arc spot movement, droplet splashing in the deposition process and the like caused by the defect of an arc control technology in the arc ion plating technology cannot be solved effectively. Researchers try to limit the movement of the arc spots by means of shielding the arc, filtering the arc and the like, or influence the movement of the arc spots by changing the arc power supply, the arc striking mode, the arc control magnetic field and the like, but the effect is not ideal. During this time, it is recognized that the most effective arc control method is magnetic field arc control, and the form of adjusting the magnitude of the magnetic field according to the motion state of the arc spot is used for controlling the motion of the arc spot. At present, various aspects of magnetic fields, arc spots, targets, including arc flows, bias voltages, atmospheres and the like are gradually researched. Through certain development, the multi-arc ion plating is practically applied to various industries such as catering utensils, sanitary ware, industrial decoration, hardware tools, steam friction light industry, medical appliances, aerospace and ordnance equipment and the like. In order to meet the field quality requirements, the requirements on the multi-arc ion plating coating are higher and higher. The coating also develops towards two or more directions of preparing a multi-component mixed coating by composite deposition of two or more materials and preparing a multi-layer structure by selecting different film materials, and researchers prepare the (Ti, cr) N mixed coating, so that the mechanical property and the corrosion resistance of the (Ti, cr) N mixed coating are superior to those of a single film coating. More researchers can prepare the (Ti, ag, cr) N mixed coating by doping Al element, and the coating performance is improved. It follows that the multiple coating is a research hotspot.
The invention patent with publication number of CN104018133B discloses a process for preparing a multilayer composite protective coating by multi-arc ion plating on the surface of a sintered neodymium-iron-boron magnet. The transition layer, the corrosion-resistant layer and the surface blocking and wear-resistant layer composite protective coating are efficiently prepared on the surface of the sintered NdFeB magnet by adopting a multi-arc ion plating deposition technology, so that the corrosion resistance of the sintered NdFeB magnet is obviously improved, and the service life is prolonged. In the invention, the AlN on the outer layer of the composite coating is formed by gas nitriding, so that the hole sealing effect is better, but the AlN has high brittleness, the coating is easy to damage, and the problem of poor surface smoothness of the coating exists.
The invention patent with publication number of CN108179385B discloses a method for preparing a wear-resistant corrosion-resistant anti-locking coating of threads by adopting multi-arc ion plating, which comprises the steps of sequentially polishing, ultrasonic cleaning and drying metal threads, then carrying out sand blasting coarsening on the dried metal threads, then carrying out sputtering cleaning to obtain surface-activated metal threads, carrying out film coating twice, firstly plating Ni as a transition layer, and carrying out secondary film coating on the metal threads with Ni transition layers on the surfaces by adopting a cathode arc source made of Ag materials and Pd materials to prepare the metal threads with Ni-AgPd coatings on the surfaces. In the process of preparing the Ni-AgPd coating on the surface of the thread by adopting multi-arc ion plating, the wear resistance of the Ni-AgPd coating is ensured by adding Pd, the thermal stability and corrosion resistance of the Ni-AgPd coating are improved, and the locking problem of a fastener is solved. However, once the coating is porous or scratched, the corrosion of the metal threads can be accelerated, the risk of locking the threads is increased, and meanwhile, the obtained coating has poor surface smoothness.
The invention patent with publication number of CN106591784B discloses a method for preparing TiAlSiCN coating by ion plating, wherein the coating adopts multi-arc ion plating as a preparation technology, a substrate is polished, cleaned by an organic solvent, dried, then ion-cleaned, then a TiN transition layer is prepared, then the TiAlSiCN coating is prepared, and the prepared TiAlSiCN coating is polished. The TiAlSiCN coating prepared by the method can solve the problem of short service life of the cutter caused by low hardness of the cutter in the machining process to a certain extent. But the coating bonds poorly to the substrate.
Disclosure of Invention
In view of the problems of poor bonding strength between the coating and the substrate, insufficient smoothness of the surface of the coating and the like in the prior art, the technical problem to be solved by the invention is to obtain the coating which has high bonding strength with the substrate, is smooth, compact, wear-resistant, corrosion-resistant, safe and antibacterial.
In order to achieve the above purpose, the invention provides a multi-arc ion plating coating process, which comprises the following steps:
step 1, pretreatment of a base material: sequentially immersing the substrate in water, absolute ethyl alcohol and acetone for 20-40 minutes by ultrasonic treatment, then drying at 45-80 ℃, and sequentially carrying out glow cleaning and metal ion bombardment to obtain a pretreated substrate for later use;
step 2, magnetically controlling the multi-arc ion plating TiN transitional coating: after the step 1, in-situ processing is carried out, a nitrogen flow valve is opened, the nitrogen flow is controlled to be 180-220 mL/min, a rotary transverse magnetic field is electrified, the magnetic field frequency and exciting current are regulated, a Ti target is electrified, the bias voltage is regulated to be 100-130V, the arc target current is 45-55A, film coating is carried out, and the film coating time is 6-10 minutes, so that the TiN transitional coating is obtained;
step 3, magnetically controlling multi-arc ion plating TiTaN coating: in-situ after the step 2, controlling the argon flow to be 50-100 mL/min, opening a nitrogen flow valve, controlling the nitrogen flow to be 100-250 mL/min, electrifying a TaTi target, adjusting the bias voltage to be 100-150V, and the arc target current to be 50-80A, and coating for 30-60 minutes to obtain TiTaN;
step 4, magnetically controlled multi-arc ion plating TiTaN-BiScCoCN composite multielement coating: in-situ after the step 3, continuously introducing argon at the speed of 50-100 mL/min, opening a nitrogen flow valve, controlling the nitrogen flow to be 100-250 mL/min, electrifying a BiScC target, adjusting the bias voltage to be 150-300V, and adjusting the arc target current to be 50-80A; the Co target is electrified, the bias voltage is regulated to 140-300V, and the arc target current is 50-60A; and (3) keeping the state for coating, wherein the coating time is 45-90 minutes, and obtaining the TiTaN-BiScCoCN composite multielement coating.
Preferably, the substrate in the step 1 is one of ferrous material, stainless steel material and ceramic material.
Preferably, the glow cleaning is to put the dried substrate into a multi-arc ion plating vacuum chamber, and vacuumize to a vacuum pressure of 1X 10 -3 ～5×10 -3 Pa, then argon with the flow rate of 100-180 mL/min is introduced, the working pressure is controlled to be 0.05-0.1 Pa, the bias voltage is regulated to be 500-1000V, and cleaning is carried out for 15-25 min.
Preferably, the target is a large-plane small-thickness round target, the size is 50-300 mm in diameter, and the thickness is 1-10 mm.
Preferably, the metal ion bombardment is performed in situ after glow cleaning, a Ti target, a TaTi target, a BiScC target and a Co target are started, a rotary transverse magnetic field is electrified, the magnetic field frequency and exciting current are regulated, and the bombardment time is 5-12 min.
Preferably, a rotary transverse magnetic field device is arranged on a flange on the side face of the target outside the multi-arc ion plating vacuum chamber, and a magnetic conduction ring is arranged around the target.
Further preferably, the rotary transverse magnetic field device consists of 24-level magnetic circuit frameworks which can regulate the voltage and the phase difference by 120 degrees and control the three-phase SPWM waveform (approximate sine wave) current, and the winding rule of 24-slot 4/2-pole delta/2Y (y=10) double-speed windings is adopted for winding embedding.
Further preferably, the rotating transverse magnetic field has a frequency of 100 to 210Hz and an excitation current of 8 to 12A.
Further, the preparation method of the BiScC target comprises the following steps of:
s1, adding 85-95 parts of high-purity bismuth and 5-15 parts of pure scandium into a crucible, vacuumizing to 0.15-0.25 Pa, smelting at 1540-1550 ℃ until metal is completely melted, maintaining a vacuum state, cooling to 700-900 ℃, uniformly stirring, pouring, cooling to 20-35 ℃ in the vacuum state, molding, taking out and sealing to obtain Bi-Sc alloy;
s2, placing 30-60 parts of the Bi-Sc alloy prepared in the step S1 and 2-10 parts of graphene into a crucible, vacuumizing to 0.15-0.25 Pa, smelting at 1540-1550 ℃ until the alloy is completely melted, maintaining the vacuum state, cooling to 400-600 ℃, uniformly stirring, adding 30-50 parts of high-purity bismuth until the bismuth is completely melted, pouring, cooling to 20-35 ℃ in the vacuum state, and forming to obtain the BiScC target.
Preferably, the pouring die in the step S1 is made of 310S stainless steel, and has a diameter of 5-10 cm and a height of 5-20 cm; and S2, the casting mold is made of 310S stainless steel, the diameter is 80-120 mm, and the thickness is 2-5 mm.
According to the invention, the substrate is pretreated, the substrate and the target are cleaned by using a glow cleaning and ion bombardment method, and then the substrate is subjected to multi-arc ion plating under a magnetic field arc control technology, so that the TiTaN-BiScCoCN composite multielement coating is obtained. And the substrate is subjected to glow cleaning and ion bombardment cleaning in sequence before multi-arc ion plating, and a magnetic field is regulated in the bombardment process, so that the surface of the substrate is etched more uniformly, and the binding force between a subsequent film coating and the substrate is improved. The magnetic field is controlled to control the uniform dispersion of the arc spots to carry out multi-arc ion plating, so that particles are thinned, and the plating layer is smoother and more compact. The coating sequence is as follows: firstly plating a TiN transition film, then plating a TiTaN coating, and finally plating a TiTaN-BiScCoCN composite multielement coating, so that the coating component is in a transition form from the substrate to the TiTaN-BiScCoCN composite multielement coating, elements at the interface of the coating are mutually diffused, and the compactness of the coating is improved. Before plating the TiTaN-BiScCoCN composite multi-element coating, starting the TaTi target to plate the TiTaN coating, wherein the Ta diffusion coefficient is small, and the TaTi target is combined with Ti and N to form an isolation layer on the surface of the substrate, so that the inter-diffusion between Bi and Sc and the substrate is reduced, the mechanical property of the substrate is prevented from being reduced, and the bonding strength between the coating and the substrate and the high-temperature oxidation resistance of the coating are further improved; in the process of plating the TiTaN-BiScCoCN composite multielement coating, the electromigration of Co is less, the perfection degree of a coating gap is improved, the coating is more compact, and meanwhile, the heat conductivity coefficient of the coating is improved by adding Co; ta and Co interact to further improve the compactness and high-temperature oxidation resistance of the coating. In addition, in the ion plating process, bi and Co are doped, so that electron migration of Bi in the coating is inhibited, the coating is more compact, and the deformation of the coating at high and low temperatures is relieved. The TiTaN-BiScCoCN composite multielement coating obtained after nitriding has stronger salt corrosion resistance and wear resistance due to the interaction of elements in ion plating.
Due to the adoption of the technical scheme, compared with the prior art, the invention has the following advantages: 1) According to the invention, the substrate is subjected to glow cleaning before multi-arc ion plating and ion bombardment under the action of a magnetic field, so that the etching of the surface of the substrate is more uniformly dispersed, and the bonding strength of a plating coating and the surface of the substrate is improved; 2) The invention adopts a large-plane small-thickness round target material, uses a magnetic field arc control technology in the multi-arc ion plating process, disperses arc spots, refines particles, and ensures that the obtained coating is smoother and denser and has better combination property with a base material; 3) In the multi-arc ion plating process, a TaTi target is firstly started to plate a TiTaN coating between a TiN transition layer and a TiTaN-BiScCoCN composite multi-element coating, so that the bonding strength between the coating and a substrate is improved, the compactness of the coating is increased, the multi-arc ion plating of a nitriding target, a BiScC target and a Co target is carried out, the compactness and the high-temperature oxidation resistance of the TiTaN-BiScCoCN composite multi-element coating are further improved, the deformation condition of the coating in high-low temperature transition is relieved, and meanwhile, the TiTaN-BiScCoCN composite multi-element coating also has good wear resistance and salt corrosion resistance.
Glow cleaning: glow cleaning, also known as glow discharge cleaning, is a relatively special vacuum system and material cleaning mode, and is generally used for cleaning and degassing in high vacuum and ultra-high vacuum systems. The desorption of the gas by electron bombardment and the removal of certain hydrocarbons can be achieved by using a hot wire or electrode as the electron source, on which a negative bias is applied with respect to the surface to be cleaned. Inert gas (such as argon, helium and the like) with proper partial pressure is required to be filled in the cleaning process, and the typical working pressure of the discharge gas is between 0.05 and 10 Pa. The inert gas is ionized in the discharging process, bombards the inner wall of the vacuum chamber and other components in the vacuum chamber, and realizes cleaning. And because of the characteristic of inert gas, the inert gas is easier to be pumped away by a vacuum system after replacing other gases adsorbed on the surface layer of the wall, thereby being beneficial to the acquisition and maintenance of ultrahigh vacuum.
Metal ion bombardment can remove contaminant layers and oxides from the substrate surface and also increase the substrate surface roughness.
Detailed Description
The raw material sources of the examples and comparative examples are as follows:
stainless steel substrate: jiangsu Hongze Metal materials Co., ltd., material: 304, thickness 1.5mm.
Ti target: beijing Decanthen metal materials science and technology Co., ltd., specification: diameter 254mm, thickness 10mm, purity: the mass fraction of Ti is more than or equal to 99.865 percent.
TaTi target: new materials, inc. Changshaxin kang, purity: 99.9, specification: diameter 50.8mm and thickness 3mm.
Co target: new materials, inc. Changshaxin kang, purity: co:99.98wt%, specification: diameter 50.8mm and thickness 3.175mm.
Graphene: shenzhen city Tuling evolution technology Co., ltd., specific surface area: 50-200 m 2 /g, particle size D 90 : 11-15 mu m, particle size D 50 : 7-12 mu m, thickness: 1-3 layers.
Example 1
A multi-arc ion plating coating process comprises the following steps:
step 1, pretreatment: immersing a stainless steel substrate with the size of 10mm multiplied by 5mm multiplied by 1.5mm in water, absolute ethyl alcohol and acetone in sequence for ultrasonic treatment for 30 minutes, then drying at 60 ℃, placing the dried substrate into a multi-arc ion coating vacuum chamber, and vacuumizing until the vacuum pressure is 3 multiplied by 10 -3 Pa, then argon with the flow of 150mL/min is introduced, the working pressure is controlled to be 0.08Pa, the starting bias voltage is 800V, the cleaning time is 20 minutes, then a Ti target, a TaTi target, a BiScC target and a Co target are started, a rotating transverse magnetic field is electrified, the frequency of the magnetic field is adjusted to be 150Hz, the exciting current is 11A, and the ion bombardment is carried out for 8 minutes, so that a pretreated substrate is obtained for standby;
step 2, magnetically controlling the multi-arc ion plating TiN transitional coating: after the step 1, in-situ processing is carried out, a nitrogen flow valve is opened, the nitrogen flow is controlled to be 200mL/min, a rotary transverse magnetic field is electrified, the frequency of the magnetic field is adjusted to be 150Hz, exciting current is 11A, a Ti target is electrified, bias voltage is adjusted to be 110V, arc target current is 50A, film coating is carried out, and film coating time is 8 minutes, so that a TiN transitional coating is obtained;
step 3, magnetically controlling multi-arc ion plating TiTaN coating: in-situ after the step 2, controlling the argon flow to be 80mL/min, opening a nitrogen flow valve, controlling the nitrogen flow to be 160mL/min, electrifying a TaTi target, adjusting the bias voltage to be 130V, and coating the film with the arc target current of 60A for 45 minutes to obtain a TiTaN coating;
step 4, magnetically controlled multi-arc ion plating TiTaN-BiScCoCN composite multielement coating: after the step 3, in-situ operation is carried out, argon is continuously introduced at 80mL/min, a nitrogen flow valve is opened, the nitrogen flow is controlled to be 160mL/min, the BiScC target is electrified, the bias voltage is adjusted to be 220V, and the arc target current is adjusted to be 70A; the Co target is electrified, the bias voltage is adjusted to 225V, and the arc target current is 55A; and (3) keeping the state for coating, wherein the coating time is 60 minutes, and obtaining the TiTaN-BiScCoCN composite multielement coating.
The preparation method of the BiScC target comprises the following steps:
s1, adding 2000g of high-purity bismuth and 222g of pure scandium into a crucible, vacuumizing to 0.2Pa, smelting at 1500 ℃ until metal is completely melted, keeping a vacuum state, cooling to 800 ℃, uniformly stirring, pouring by using a die with the diameter of 8cm and the height of 15cm, cooling to 25 ℃ in the vacuum state, molding, taking out and sealing to obtain Bi-Sc alloy;
s2, placing 889g of the Bi-Sc alloy prepared in the step S1 and 111g of graphene into a crucible, vacuumizing to 0.2Pa, smelting at 1545 ℃ until the alloy is completely melted, maintaining the vacuum state, cooling to 500 ℃, uniformly stirring, adding 1111g of high-purity bismuth until the bismuth is completely melted, pouring with a die with the diameter of 100mm and the height of 3mm, cooling to 25 ℃ in the vacuum state, and forming to obtain the BiScC target.
Comparative example 1
A multi-arc ion plating coating process comprises the following steps:
step 1, pretreatment: immersing a stainless steel substrate with the size of 10mm multiplied by 5mm multiplied by 1.5mm in water, absolute ethyl alcohol and acetone in sequence for ultrasonic treatment for 30 minutes, then drying at 60 ℃, placing the dried substrate into a multi-arc ion coating vacuum chamber, and vacuumizing until the vacuum pressure is 3 multiplied by 10 -3 Pa, then argon with the flow rate of 150mL/min is introduced, the working pressure is controlled to be 0.08Pa, the starting bias voltage is 800V, the cleaning time is 20 minutes, then a Ti target, a BiScC target and a Co target are started, a rotating transverse magnetic field is electrified, the frequency of the magnetic field is adjusted to be 150Hz, the exciting current is 11A, and the ion bombardment is carried out for 8 minutes, so that a pretreated substrate is obtained for standby;
step 2, magnetically controlling the multi-arc ion plating TiN transitional coating: after the step 1, in-situ processing is carried out, a nitrogen flow valve is opened, the nitrogen flow is controlled to be 200mL/min, a rotary transverse magnetic field is electrified, the frequency of the magnetic field is adjusted to be 150Hz, exciting current is 11A, a Ti target is electrified, bias voltage is adjusted to be 110V, arc target current is 50A, film coating is carried out, and film coating time is 8 minutes, so that a TiN transitional coating is obtained;
step 3, magnetically controlled multi-arc ion plating TiN-BiScCoCN composite multielement coating: in-situ after the step 2, continuously introducing argon at 80mL/min, opening a nitrogen flow valve, controlling the nitrogen flow to 160mL/min, electrifying a BiScC target, adjusting the bias voltage to 220V, and adjusting the arc target current to 70A; the Co target is electrified, the bias voltage is adjusted to 225V, and the arc target current is 55A; and (3) keeping the state for coating, wherein the coating time is 60 minutes, and obtaining the TiN-BiScCoCN composite multielement coating.
The BiScC target preparation method was the same as in example 1.
Comparative example 2
A multi-arc ion plating coating process comprises the following steps:
step 1, pretreatment: immersing a stainless steel substrate with the size of 10mm multiplied by 5mm multiplied by 1.5mm in water, absolute ethyl alcohol and acetone in sequence for ultrasonic treatment for 30 minutes, then drying at 60 ℃, placing the dried substrate into a multi-arc ion coating vacuum chamber, and vacuumizing until the vacuum pressure is 3 multiplied by 10 -3 Pa, then argon with the flow rate of 150mL/min is introduced, the working pressure is controlled to be 0.08Pa, the starting bias voltage is 800V, the cleaning time is 20 minutes, then a Ti target, a TaTi target and a BiScC target are started, a rotating transverse magnetic field is electrified, the frequency of the magnetic field is adjusted to be 150Hz, the exciting current is 11A, and the ion bombardment is carried out for 8 minutes, so that a pretreated substrate is obtained for standby;
step 2, magnetically controlling the multi-arc ion plating TiN transitional coating: after the step 1, in-situ processing is carried out, a nitrogen flow valve is opened, the nitrogen flow is controlled to be 200mL/min, a rotary transverse magnetic field is electrified, the frequency of the magnetic field is adjusted to be 150Hz, exciting current is 11A, a Ti target is electrified, bias voltage is adjusted to be 110V, arc target current is 50A, film coating is carried out, and film coating time is 8 minutes, so that a TiN transitional coating is obtained;
step 3, magnetically controlling multi-arc ion plating TiTaN coating: in-situ after the step 2, controlling the argon flow to be 80mL/min, opening a nitrogen flow valve, controlling the nitrogen flow to be 160mL/min, electrifying a TaTi target, adjusting the bias voltage to be 130V, and coating the film with the arc target current of 60A for 45 minutes to obtain a TiTaN coating;
step 4, magnetically controlled multi-arc ion plating TiTaN-BiScCN composite multielement coating: and 3, continuously introducing argon at 80mL/min, opening a nitrogen flow valve, controlling the nitrogen flow to 160mL/min, electrifying a BiScC target, adjusting the bias voltage to 220V, keeping the arc target current to 70A, and coating for 60 minutes to obtain the TiTaN-BiScCN composite multielement coating.
The BiScC target preparation method was the same as in example 1.
Comparative example 3
A multi-arc ion plating coating process comprises the following steps:
step 1, pretreatment: immersing a stainless steel substrate with the size of 10mm multiplied by 5mm multiplied by 1.5mm in water, absolute ethyl alcohol and acetone in sequence for ultrasonic treatment for 30 minutes, then drying at 60 ℃, placing the dried substrate into a multi-arc ion coating vacuum chamber, and vacuumizing until the vacuum pressure is 3 multiplied by 10 -3 Pa, then argon with the flow rate of 150mL/min is introduced, the working pressure is controlled to be 0.08Pa, the starting bias voltage is 800V, the cleaning time is 20 minutes, then a Ti target, a TaTi target and a Co target are started, a rotating transverse magnetic field is electrified, the frequency of the magnetic field is adjusted to be 150Hz, the exciting current is 11A, and the ion bombardment is carried out for 8 minutes, so that a pretreated substrate is obtained for standby;
step 2, magnetically controlling the multi-arc ion plating TiN transitional coating: after the step 1, in-situ processing is carried out, a nitrogen flow valve is opened, the nitrogen flow is controlled to be 200mL/min, a rotary transverse magnetic field is electrified, the frequency of the magnetic field is adjusted to be 150Hz, exciting current is 11A, a Ti target is electrified, bias voltage is adjusted to be 110V, arc target current is 50A, film coating is carried out, and film coating time is 8 minutes, so that a TiN transitional coating is obtained;
step 3, magnetically controlling multi-arc ion plating TiTaN coating: in-situ after the step 2, controlling the argon flow to be 80mL/min, opening a nitrogen flow valve, controlling the nitrogen flow to be 160mL/min, electrifying a TaTi target, adjusting the bias voltage to be 130V, and coating the film with the arc target current of 60A for 45 minutes to obtain a TiTaN coating;
step 4, magnetically controlled multi-arc ion plating TiTaN-CoN composite multielement coating: and 3, in-situ processing is carried out after the step 3, argon is continuously introduced at 80mL/min, a nitrogen flow valve is opened, the nitrogen flow is controlled to be 160mL/min, a Co target is electrified, the bias voltage is adjusted to be 225V, the arc target current is 55A, the state is kept for film coating, and the film coating time is 60 minutes, so that the TiTaN-CoN composite multielement coating is obtained.
Comparative example 4
A multi-arc ion plating coating process comprises the following steps:
step 1, pretreatment: immersing the stainless steel substrate with the size of 10mm multiplied by 5mm multiplied by 1.5mm in water, absolute ethyl alcohol and acetone in turnSound for 30 minutes, then drying at 60 ℃, putting the dried base material into a multi-arc ion coating vacuum chamber, vacuumizing until the vacuum pressure is 3 multiplied by 10 -3 Pa, then argon with the flow of 150mL/min is introduced, the working pressure is controlled to be 0.08Pa, the starting bias voltage is 800V, the cleaning time is 20 minutes, then a Ti target, a TaTi target, a BiScC target and a Co target are started, a rotating transverse magnetic field is electrified, the frequency of the magnetic field is adjusted to be 150Hz, the exciting current is 11A, and the ion bombardment is carried out for 8 minutes, so that a pretreated substrate is obtained for standby;
step 2, magnetically controlling the multi-arc ion plating TiN transitional coating: after the step 1, in-situ processing is carried out, a nitrogen flow valve is opened, the nitrogen flow is controlled to be 200mL/min, a rotary transverse magnetic field is electrified, the frequency of the magnetic field is adjusted to be 150Hz, exciting current is 11A, a Ti target is electrified, bias voltage is adjusted to be 110V, arc target current is 50A, film coating is carried out, and film coating time is 8 minutes, so that a TiN transitional coating is obtained;
step 3, magnetically controlling the multi-arc ion plating TiCoN coating: 2, in-situ processing is carried out after the step, wherein the argon flow is controlled to be 80mL/min, a nitrogen flow valve is opened, the nitrogen flow is controlled to be 160mL/min, a Co target is electrified, the bias voltage is adjusted to be 225V, the arc target current is 55A, film coating is carried out, and the film coating time is 45 minutes, so that a TiTaN coating is obtained;
step 4, magnetically controlled multi-arc ion plating TiCoN-BiScTaCN composite multielement coating: after the step 3, in-situ operation is carried out, argon is continuously introduced at 80mL/min, a nitrogen flow valve is opened, the nitrogen flow is controlled to be 160mL/min, the BiScC target is electrified, the bias voltage is adjusted to be 220V, and the arc target current is adjusted to be 70A; the TiTa target is electrified, the bias voltage is adjusted to be 130V, and the arc target current is 60A; and (3) keeping the state for coating, wherein the coating time is 60 minutes, and obtaining the TiCoN-BiScTaCN composite multielement coating.
The BiScC target preparation method was the same as in example 1.
Test example 1
Coating and substrate binding force test:
referring to the doctor paper (performance research of tantalum-based nanocrystalline coating in simulated biological environment, author: liu Linlin, university of aviation aerospace in Nanj, 2017), a method for measuring binding force by adopting scratch experiment is used for testing binding force between a coating sample and a substrate by using a Nano indentation instrument with the model of Nano indicator G200, and the test conditions are as follows: the maximum load was set at 80mN, the scratch speed was 10 μm/s, the scratch length was 500 μm, the vertical load applied to the press head during the scratching was increased from 30 μm to the set maximum load of 80mN, the change in the acoustic emission signal of the instrument was monitored, and when the acoustic emission signal suddenly increased, the occurrence of peeling of the coating was indicated, and the load at this time was the critical load Lc, showing the bonding strength between the coating and the substrate, and the results are shown in table 1.
Test example 2
Coating abrasion resistance test:
the friction performance test was carried out on an MS-T3000 friction abrasion tester with reference to journal paper (performance study of multi-arc ion plating ZrN plating on stainless steel surface, author: rao Xiaoxiao et al, metal materials and metallurgical engineering, 2021), the coating sample was fixed on a test platform, a 30-minute rolling friction type opposite abrasion test was carried out with a 45-steel ring, the weight of the sample before and after abrasion was weighed, and the abrasion condition was represented by the mass loss meter of the sample before and after abrasion, and the results are shown in Table 1.
Test example 3
Coating hot salt corrosion resistance test:
referring to the master paper (preparation of multi-arc ion plating NiSiAlY coating and study on hot salt corrosion performance, author: cui Tian, national institute of science and engineering, 2020), hot salt corrosion test was performed on a coating sample, the test steps were: 1) Brushing salt on the surface of the coating sample and drying at 45 ℃ to obtain the coating with the salt content of 5mg/cm 2 The method comprises the steps of carrying out a first treatment on the surface of the 2) The muffle furnace was heated to 600 ℃, the coating sample of step 1) was placed in a clean crucible, then placed in the muffle furnace at 600 ℃ for 4 hours, and the corrosion condition of the coating surface was observed, and the results are shown in table 1, wherein the corrosion condition is obvious, slight corrosion and no corrosion.
TABLE 1 coating Performance test results
( Remarks: the more severe the scratch, the worse the binding force between the coating and the substrate; the less the scratch, the better the coating bonds to the substrate. The smaller the abrasion amount is, the better the abrasion resistance is; the larger the amount of wear, the poorer the wear resistance. )
As can be seen from the comparison of the example 1 and the comparative examples 1 to 3, the binding force, the wear resistance and the salt corrosion resistance of the coating of the example 1 are all better than those of the comparative examples 1 to 3, probably because in the example 1, the substrate is etched before the coating, so that the surface roughness of the substrate is increased and the coating is uniformly dispersed, and the coating and the substrate are better combined during the ion coating; during film coating, the TaTi target is firstly started, then the BiScC target and the Co target are started, and nitrogen, ta, co, bi and other element ions are introduced to interact, so that the coating is more compact and wear-resistant, the bonding strength of the coating and a substrate is further improved, and meanwhile, the hot salt corrosion resistance of the coating is also improved.
Claims (9)
1. The multi-arc ion plating film coating process is characterized by comprising the following steps of:
step 1, pretreatment of a base material: sequentially immersing the substrate in water, absolute ethyl alcohol and acetone for 20-40 minutes by ultrasonic treatment, then drying at 45-80 ℃, and sequentially carrying out glow cleaning and metal ion bombardment to obtain a pretreated substrate for later use;
step 2, magnetically controlling the multi-arc ion plating TiN transitional coating: after the step 1, performing in-situ operation, namely opening a nitrogen flow valve, controlling the nitrogen flow to be 180-220 mL/min, electrifying a rotary transverse magnetic field, adjusting the magnetic field frequency and exciting current, electrifying a Ti target, adjusting the bias voltage to be 100-130V, adjusting the arc target current to be 45-55A, and performing coating for 6-10 minutes to obtain a TiN transitional coating;
step 3, magnetically controlling multi-arc ion plating TiTaN coating: 2, in-situ processing is carried out after the step, the argon flow is controlled to be 50-100 mL/min, a nitrogen flow valve is opened, the nitrogen flow is controlled to be 100-250 mL/min, a TaTi target is electrified, the bias voltage is regulated to be 100-150V, the arc target current is 50-80A, film coating is carried out, and the film coating time is 30-60 minutes, so that TiTaN is obtained;
step 4, magnetically controlling multi-arc ion plating of BiScCoCN coating: in-situ after the step 3, continuously introducing argon at the speed of 50-100 mL/min, opening a nitrogen flow valve, controlling the nitrogen flow to be 100-250 mL/min, electrifying a BiScC target, adjusting the bias voltage to be 150-300V, and adjusting the arc target current to be 50-80A; the Co target is electrified, the bias voltage is adjusted to 140-300V, and the arc target current is 50-60A; and (5) keeping the state for coating, wherein the coating time is 45-90 minutes, and obtaining the BiScCoCN coating.
2. A multi-arc ion plating coating process according to claim 1, wherein: the base material is one of an iron material, a stainless steel material and a ceramic material.
3. The multi-arc ion plating coating process of claim 1, wherein the preparation method of the BiScC target comprises the following steps of:
s1, adding 85-95 parts of high-purity bismuth and 5-15 parts of pure scandium into a crucible, vacuumizing to 0.15-0.25 Pa, smelting at 1540-1550 ℃ until metal is completely melted, maintaining a vacuum state, cooling to 700-900 ℃, uniformly stirring, casting, cooling to 20-35 ℃ in the vacuum state, molding, taking out and sealing to obtain Bi-Sc alloy;
s2, placing 30-60 parts of the Bi-Sc alloy prepared in the step S1 and 2-10 parts of graphene into a crucible, vacuumizing to 0.15-0.25 Pa, smelting at 1540-1550 ℃ until the alloy is completely melted, maintaining a vacuum state, cooling to 400-600 ℃, uniformly stirring, adding 30-50 parts of high-purity bismuth until the bismuth is completely melted, casting, cooling to 20-35 ℃ in the vacuum state, and forming to obtain the BiScC target.
4. A multi-arc ion plating coating process according to claim 3, wherein: the casting die is made of 310S stainless steel, the diameter of the casting die is 5-10 cm, and the height of the casting die is 5-20 cm; and step S2, the casting mold is made of 310S stainless steel, the diameter is 80-120 mm, and the thickness is 2-5 mm.
5. A multi-arc ion plating coating process according to claim 2, wherein: and the glow cleaning is to put the dried substrate into a multi-arc ion plating vacuum chamber, vacuumize the chamber until the vacuum pressure is 1 multiplied by 10 < -3 > to 5 multiplied by 10 < -3 > Pa, then introduce argon with the flow of 100 to 180mL/min, control the working pressure to be 0.05 to 0.1Pa, start the bias voltage to be-1000 to-500V, and clean the substrate for 15 to 25min.
6. A multi-arc ion plating coating process according to claim 2, wherein: the target material is a large-plane small-thickness round target material, the size is 50-300 mm in diameter, and the thickness is 1-10 mm.
7. A multi-arc ion plating coating process according to claim 2, wherein: the metal ion bombardment is performed in situ after glow cleaning, a Ti target, a TaTi target, a BiScC target and a Co target are started, a rotary transverse magnetic field is electrified, the magnetic field frequency and exciting current are regulated, and the bombardment time is 5-12 min.
8. A multi-arc ion plating coating process according to claim 2, wherein: the frequency of the rotating transverse magnetic field is 100-210 Hz, and the exciting current is 8-12A.
9. A composite multi-component coating of a TiTaN-BiScCoCN, which is characterized in that: the multi-arc ion plating coating process according to any one of claims 1 to 8.
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