CN114164405B - Tool thick film nitride coating and preparation method thereof - Google Patents
Tool thick film nitride coating and preparation method thereof Download PDFInfo
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- CN114164405B CN114164405B CN202111485551.8A CN202111485551A CN114164405B CN 114164405 B CN114164405 B CN 114164405B CN 202111485551 A CN202111485551 A CN 202111485551A CN 114164405 B CN114164405 B CN 114164405B
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- 239000011248 coating agent Substances 0.000 title claims abstract description 120
- 150000004767 nitrides Chemical class 0.000 title claims abstract description 45
- 238000002360 preparation method Methods 0.000 title claims abstract description 14
- 238000001704 evaporation Methods 0.000 claims abstract description 38
- 238000000034 method Methods 0.000 claims abstract description 32
- 238000005516 engineering process Methods 0.000 claims abstract description 27
- 238000007733 ion plating Methods 0.000 claims abstract description 27
- 238000007747 plating Methods 0.000 claims abstract description 21
- 230000007704 transition Effects 0.000 claims abstract description 20
- 239000013077 target material Substances 0.000 claims abstract description 19
- 238000000151 deposition Methods 0.000 claims abstract description 16
- 230000008021 deposition Effects 0.000 claims abstract description 16
- 229910017150 AlTi Inorganic materials 0.000 claims abstract description 8
- 150000001875 compounds Chemical class 0.000 claims abstract description 7
- 230000008020 evaporation Effects 0.000 claims description 26
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 18
- 238000004140 cleaning Methods 0.000 claims description 14
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- 229910052757 nitrogen Inorganic materials 0.000 claims description 9
- 238000005530 etching Methods 0.000 claims description 7
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- 238000005240 physical vapour deposition Methods 0.000 description 10
- 238000005520 cutting process Methods 0.000 description 9
- 238000005229 chemical vapour deposition Methods 0.000 description 8
- 239000010409 thin film Substances 0.000 description 8
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- 238000007740 vapor deposition Methods 0.000 description 6
- 238000001755 magnetron sputter deposition Methods 0.000 description 5
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 description 4
- 239000007888 film coating Substances 0.000 description 4
- 238000009501 film coating Methods 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- 229910000997 High-speed steel Inorganic materials 0.000 description 3
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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
-
- 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
- C23C14/14—Metallic material, boron or silicon
- C23C14/16—Metallic material, boron or silicon on metallic substrates or on substrates of boron or silicon
-
- 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
- C23C14/58—After-treatment
- C23C14/5846—Reactive treatment
- C23C14/586—Nitriding
Landscapes
- 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 thick film nitride coating of a cutter and a preparation method thereof. The preparation method adopts vacuum cathode arc ion plating technology to carry out film plating, and is assisted by ion source assisted deposition technology and/or pulse magnetic field or direct current magnetic field; firstly, evaporating a Cr target material in Ar atmosphere to form a Cr transition layer film on the surface of a cutter, and then, forming a Cr transition layer film on the surface of the cutter in N 2 Evaporating the multi-element compound target material under atmosphere to form multi-element nitride film with thickness of 7.5-10 μm, and finally forming the multi-element nitride film in N 2 Evaporating the AlTi target material in the atmosphere to form the AlTiN film. The invention effectively improves the thickness of the cutter coating prepared by the vacuum cathode arc ion plating process, and greatly improves the comprehensive performance of the coating and the service life of the cutter.
Description
Technical Field
The invention relates to the technical field of cutter coatings, in particular to a cutter thick film nitride coating and a preparation method of the cutter thick film nitride coating.
Background
Vapor deposition is a technique that uses physical and chemical reaction processes occurring in a vapor phase to change the surface composition of parts to form a metal or compound coating having a specific function on the surface. Vapor deposition can be categorized into two general categories, chemical Vapor Deposition (CVD) and Physical Vapor Deposition (PVD) by the nature of the process.
The application of vapor deposition technology relates to various fields, and the application of the vapor deposition technology is very wide only in the aspect of improving the wear resistance and corrosion resistance of mechanical parts. The coating such as TiN, tiC, ti (CN) and the like prepared by the vapor deposition technology has very high hardness and wear resistance, so that the plating of the TiN film on the high-speed steel tool is a revolution of the high-speed steel tool, and the service life of the tool can be prolonged by more than 3 times by plating the TiN film with the thickness of 1-3 mu m on the cutting surface of the tool.
Chemical Vapor Deposition (CVD) is a process of chemically reacting a gaseous substance at a certain temperature on a solid surface and forming a solid deposition film on the surface thereof. Physical Vapor Deposition (PVD) is a process in which a metal, alloy, or compound is vaporized in a vacuum chamber to deposit the vapor atoms or molecules onto the surface of a workpiece under certain conditions. Compared with CVD, PVD has the main advantages of lower treatment temperature, higher deposition speed, no pollution and the like, thus having high practical value. The PVD has the defects that the binding force between the coating and the workpiece is low, the thickness of the coating is thin, and particularly, the defects are more remarkable along with the gradual increase of the hardness of the coating, so that the service life of a coated cutter is further influenced. Table 1 lists a comparison of PVD and CVD coating processes and characteristics.
Table 1 comparison of PVD and CVD coating processes and characteristics
Vacuum cathodic arc ion plating, which is called multi-arc ion plating or multi-arc plating if two or more vacuum arc evaporation sources are used, is called vacuum arc ion plating for short, which belongs to PVD coating technology. Vacuum cathodic arc ion plating is a vacuum ion plating technique using vacuum arc discharge as evaporation source, and has been widely used for coating of tools and dies, including TiN, tiCN, tiAlN, al 2 O 3 、AlCrN、MoS 2 Film series such as WC/C.
Vacuum cathodic arc ion plating has the following advantages:
(1) The evaporation source is a solid cathode target, plasma is directly generated from the cathode target source, and the arc target source can be arranged in any direction and multiple sources to ensure uniform coating;
(2) The device has a simpler structure, the arc target source is not only an evaporation source of cathode materials, but also an ion source, and only reaction gas exists when reactive deposition is carried out, so that the atmosphere is simple to control;
(3) The ionization rate is high, generally up to 60% -80%, the deposition rate is high, and the method is a main tool coating preparation means at present;
(4) The incident ion energy is high, the internal stress of the film is relatively low, and the film base binding force is good;
(5) The low-voltage power supply is adopted for working, and the production is safer.
The disadvantages of vacuum cathodic arc ion plating are also apparent. In the aspect of turning tools, the thickness of the coating is indistinguishable from the service life of the tools, the thickness of the conventional coating of the vacuum cathode arc ion plating is smaller than 5 mu m and is far lower than 20 mu m of CVD, and therefore, the application of PVD coating in the aspect of turning is greatly restricted. The thickness of the vacuum cathode arc ion plating coating determines the performance of the coating, and how to increase the thickness of the vacuum cathode arc ion plating coating is a key technology for prolonging the service life of a coated cutter.
Disclosure of Invention
The technical problems to be solved by the invention are as follows: the thick film nitride coating for the cutter with the thicker thickness can effectively prolong the service life of the cutter.
The technical scheme adopted by the invention for solving the technical problems is as follows: the thick film nitride coating of the cutter is a multi-element multi-layer coating which is formed by plating a Cr layer, a multi-element nitride layer and an AlTiN layer on the surface of the cutter from inside to outside.
Further is: the multi-element nitride layer is an AlCrSiN layer, an AlCrWN layer or an AlTiCrSiN layer.
The invention also discloses a method for preparing the thick film nitride coating of the cutter, which adopts a vacuum cathode arc ion plating technology to carry out film plating, and is assisted by an ion source assisted deposition technology and/or a pulse magnetic field or a direct current magnetic field; firstly, evaporating a Cr target material in Ar atmosphere to form a Cr transition layer film on the surface of a cutter, and then, forming a Cr transition layer film on the surface of the cutter in N 2 Evaporating the multi-element compound target material under atmosphere to form multi-element nitride film with thickness of 7.5-10 μm, and finally forming the multi-element nitride film in N 2 Evaporating the AlTi target material in the atmosphere to form the AlTiN film.
Further is: the method comprises the following steps:
A. pre-treating the cutter;
B. vacuumizing the vacuum chamber and preheating;
C. glow cleaning;
D. the vacuum chamber is vacuumized and preheated;
E. etching by an ion source;
F. plating films, namely sequentially plating a Cr transition layer film, a multi-element nitride transition film, a multi-element nitride film and an AlTiN film by adopting a vacuum cathode arc ion plating technology, wherein the number and the movement speed of arc spots are increased by adopting a pulse magnetic field or direct current magnetic field technology in the process of plating the films;
G. and (5) cooling.
Further is: the method comprises the following steps:
A. cleaning and drying the cutter;
B. vacuumizing the vacuum chamber and preheating to 400 ℃;
C. the pressure of the vacuum chamber is emphasized to 2.0Pa, ar gas with the flow of 120-240 sccm is fed, a bias power supply is started, the bias voltage is-500-1000V, and glow cleaning is carried out for 5-10 min;
D. closing a bias power supply, vacuumizing to 0.005Pa, and preheating to 550 ℃;
E. starting an ion source, wherein the power of the ion source is 1.0-3.0 kw, starting a bias power supply, the bias voltage is-300 to-400V, feeding Ar gas with the flow of 40-80 sccm, and etching for 40-60 min;
F. firstly, starting a Cr cathode evaporation source, an arc power supply 80-90A, a pulse magnetic field voltage 0V, a bias voltage direct current 80-100V, and a coating time 5-10 min; then starting the multi-compound cathode evaporation source, and firstly adjusting the control parameters as follows: arc current 80-90A, pulse magnetic field voltage 10-20V, pulse frequency 33.3-66.7 Hz, DC magnetic field voltage 0.5-2.0V, nitrogen flow 600-800 sccm, bias voltage-50-100V, bias voltage increasing in coating period, coating period 5-15 min; the control parameters are then adjusted as: arc current 80-90A, pulse magnetic field voltage 15-30V, pulse frequency 11.1-33.3 Hz, direct current magnetic field voltage 1.5-3.0V, nitrogen flow 600-800 sccm, bias voltage-100-50V, bias voltage decreasing in the coating period, starting ion source and/or sputtering source, ion source power 0.5-1.5 kw, sputtering source power 1-2 kw, coating time 180-360 min; finally, starting an AlTi cathode evaporation source, wherein the arc current is 80-100A, the pulse magnetic field voltage is 15-30V, the pulse frequency is 11.1-16.7 Hz, the direct current magnetic field voltage is 0.5-1.5V, the nitrogen flow is 500-700 sccm, the bias voltage is-50 to-130V, the bias voltage is increased gradually in the coating period, and the coating time is 20-40 min;
G. cooling for 120-150 min after coating.
Further is: the thickness of the Cr transition layer film is 100-200 nm; the AlTiN film has a thickness of 0.3 to 0.7 μm.
The beneficial effects of the invention are as follows: the invention improves the vacuum cathode arc ion plating process, increases the number and the movement speed of target arc spots by using a pulse magnetic field or a direct current magnetic field to improve nucleation density, inhibits the increase of film growth stress by using an ion source auxiliary deposition technology, and improves the density of critical atomic groups in unit area by regulating and controlling the frequency of the pulse magnetic field of the cathode arc.
Drawings
FIG. 1 is a ball mark morphology of a thick film nitride coating for a tool prepared in accordance with the present invention;
FIG. 2 is a chart of the base film hardness of a Cr/AlTiCrSiN/AlTiN coating prepared according to the present invention;
FIG. 3 is a chart of the hardness of an interlayer of a Cr/AlTiCrSiN/AlTiN coating prepared according to the present invention;
FIG. 4 is a chart of the surface hardness of a Cr/AlTiCrSiN/AlTiN coating prepared according to the present invention;
FIG. 5 is a graph of the scratch test results for Cr/AlCrWN/AlTiN coatings prepared according to the present invention.
Detailed Description
In order to facilitate the understanding of the present invention, the present invention will be further described with reference to the accompanying drawings and examples.
In the vacuum cathodic arc ion plating process, the reasons for restricting the increase of the coating thickness can be summarized as: nucleation, film growth, film texture, and internal stress generation of the film.
And (3) nucleation:
new core formation is required during the initial stages of the deposition process. The method for obtaining the flat and uniform film needs to increase the density N of critical atomic groups in unit area and reduce the interfacial energy r in unit area. In the deposition nucleation stage, the supersaturation degree of the gas phase can be greatly improved to form a thin film with fine core and compactness and continuity. When the gas phase saturation is increased to a certain degree, the gas phase saturation is reduced to a small degree, and meanwhile, the difference delta G between the free energy of phase change in the condensation process is also greatly reduced, so that the nucleation rate of the film can be improved.
Film growth:
the film growth process comprises the following three processes: deposition or adsorption of gas phase atoms, surface diffusion, bulk diffusion.
Since these processes are all controlled by the activation energy of the process, the formation of the thin film structure will be closely related to the relative substrate temperature Ts/Tm (melting point temperature) at the time of deposition and the energy of the deposited atoms themselves.
The structure of the film can be four kinds according to the deposition conditions:
form 1: exhibiting a fine fibrous morphology
Form T: transition type tissue between form 1 and form 2
Form 2: presenting columnar crystal structure
Form 3: grain epitaxial structure exhibiting coarse equiaxed crystal
Texture tendency of the film:
crystalline films often have a certain tendency to texture. In many cases it is desirable to have a specific texture to enhance the properties of the film. The surface energy of the crystal is different in all directions, i.e. it is anisotropic. During thin film deposition, it results in a thin film deposition rate that varies with crystallographic orientation.
The formation process of the film texture is the process of competing growth of grains with various orientations, the grains with low growth speed are covered by other grains, and the crystallographic direction with the highest growth speed becomes the texture direction of the film.
Stress of the film:
the stress in the thin film can be classified into thermal stress and growth stress according to the root cause of the stress generated in the thin film.
In the case of temperature change, the internal stress of the film due to the expansion and contraction effect of the constrained film is a thermal stress. The film is always attached to the substrate material and, due to the difference in linear expansion coefficients between the substrate and the film, causes the substrate and the film to have different tendencies to expand and contract during the heat treatment. And in the case of mutual constraints at the interface, stresses and deformations are induced in the surface and the substrate.
Intrinsic stress of a film refers to internal stress of the film due to unbalance of the film structure. The preparation of thin film materials often involves certain unbalanced processes such as deposition of thin films at relatively low temperatures, bombardment of energetic particles, inclusion of gas and impurity atoms, relatively large temperature gradients, the presence of large numbers of defects and voids, the creation of metastable or amorphous phases, etc., which all cause the state of the structure of the thin film material to deviate from equilibrium and, in response thereto, leave stresses in the thin film. This stress due in part to the nature of the film deposition process is referred to as the growth stress.
For vacuum cathodic arc ion plating, the thickness of the coating prepared by the vacuum cathodic arc ion plating technology is about 2-4 mu m, the increase of the thickness of the coating is beneficial to the improvement of the wear resistance of the coating, and the service life of the cutting tool is influenced by the wear resistance of the coating for turning cutting tools; although the current magnetron sputtering technology can prepare a coating with the thickness of more than 10 mu m, the size of the coating crystal grain is more than 100nm, and the coating has a typical columnar crystal structure, so that the bonding degree between the coating and a cutter substrate is poor and the stability is poor.
The invention starts from the reason of restricting the thickness increase of the coating, aims at the problems of nucleation, film growth, film texture and internal stress of the film in the film plating process of the vacuum cathode arc ion plating technology, realizes the preparation of the thick film coating by improving the vacuum cathode arc ion plating technology process, ensures that the thickness of the thick film nitride coating of the prepared cutter reaches 6-10 mu m, breaks through the range restriction of 2-4 mu m of the thickness of the coating prepared by the traditional vacuum cathode arc ion plating technology, and greatly prolongs the service life of the coating.
Because the high-speed friction between the cutter and the workpiece makes the cutter in a high-temperature condition when the cutter performs processing work, the cutting force is large, the cutting temperature is high, the work hardening is serious, which is an important influencing factor for influencing the service performance and the service life of the cutter, and the thermal stability of the cutter coating is the most important factor for influencing the comprehensive performance of the cutter coating under the high-temperature condition. The traditional cutter adopts a coating which is mainly a TiAlN coating and an AlCrN coating, the TiAlN coating can be decomposed and separated into fcc-AlN phases of a face-centered cubic structure through amplitude modulation under the high temperature condition, the fcc-AlN phases are gradually converted into hcp-AlN phases of a close-packed hexagonal structure, and the hardness of the cutter coating is reduced due to the generation of soft hcp-AlN phases, so that the function of the TiAlN coating is attenuated; while AlCrN coatings also present similar problems.
The thick film nitride coating of the cutter disclosed by the invention is a multi-element multi-layer coating which is formed by plating a Cr layer, a multi-element nitride layer and an AlTiN layer on the surface of the cutter from inside to outside. Wherein the multi-element nitride layer is AlCrSiN layer, alCrWN layer or AlTiCrSiN layer. Because Cr has good ductility and coverage and good bonding property with steel parts and hard alloy materials, the Cr layer is used as a transition film layer, and the aim of relieving the thermal stress between film bases is fulfilled by the characteristics of the Cr film. The thick film nitride coating of the tool disclosed by the invention forms a single nano grain structure phase mainly comprising AlTiN or AlCrN, and has (111) and (200) double orientation characteristics on an XRD diffraction pattern, the grain size is 20-40 nm, and the film hardness can be improved by about 10% compared with that of a conventional coating. The multi-element nitride layer plated by the multi-element material in the coating is beneficial to regulating and controlling the texture tendency of the film, for example, the addition of Si element in the multi-element nitride layer can refine the grain size and reduce the texture strength of the film, thereby reducing the growth stress of the film and promoting the increase of the thickness of the coating.
The thick film nitride coating of the cutter disclosed by the invention adopts a vacuum cathode arc ion plating technology to carry out film plating, and is assisted by an ion source assisted deposition technology and/or a pulse magnetic field or a direct current magnetic field; in the preparation, cr is first evaporated under Ar atmosphereForming a Cr transition layer film with the thickness of 100-200 nm on the surface of the cutter by the target material, and then forming a Cr transition layer film with the thickness of 100-200 nm on the surface of the cutter by the target material 2 Evaporating the multi-element compound target material under atmosphere to form multi-element nitride film with thickness of 7.5-10 μm, and finally forming the multi-element nitride film in N 2 Evaporating the AlTi target material under the atmosphere to form the AlTiN film with the thickness of 0.3-0.7 mu m.
When the preparation of the thick film nitride coating of the cutter is carried out, the preparation method comprises the following process steps:
A. the method comprises the steps of preprocessing a cutter, wherein the preprocessing of the cutter comprises the steps of cleaning and drying the cutter and checking coating equipment, so that the cleanliness of the surface of the cutter needs to be ensured, and the follow-up coating work is facilitated;
B. vacuumizing and preheating the vacuum chamber, wherein the vacuum environment of the vacuum chamber of the coating equipment is ensured;
C. glow cleaning, wherein the step slows down the discharge intensity of the subsequent ion source etching through glow discharge cleaning, thereby achieving the purpose of protecting the cutter;
D. the vacuum chamber is vacuumized and preheated;
E. ion source etching, wherein ions are used for bombarding the surface of a workpiece to be plated to realize the cleaning work of the surface of the workpiece, and the ion etching has lower damage degree to the surface of the workpiece in the cleaning process, so that the thorough cleaning and activation of the surface of the workpiece can be simultaneously realized;
F. coating, namely sequentially coating a Cr transition layer film, a multi-nitride transition film, a multi-nitride film and an AlTiN film by adopting a vacuum cathode arc ion plating technology, evaporating a target material by adopting the vacuum cathode arc ion plating technology in a coating process, and increasing the number of arc spots and the movement speed by adopting a pulse magnetic field or direct current magnetic field technology; in the initial stage of plating the multi-element nitride transition film, the density of critical atomic groups in unit area is improved by increasing the frequency of a cathodic arc pulse magnetic field, so that a flat and uniform basic bottom film is obtained; in the stage of plating the multi-element nitride film, the ion source and/or the magnetron sputtering source are utilized to interfere and control the growth of film grains through a plasma auxiliary deposition technology, so that the increase of the growth stress of the film is inhibited, and the overall thickness of the coating is increased to prolong the service life of the coating;
the coating temperature is controlled in the coating stage, so that the coating temperature is not lower than 550 ℃, and the regulation and control of the grain structure are facilitated; the traditional vacuum cathode arc ion plating technology can splash fine liquid drops from the surface of a target during deposition, the liquid drops are condensed in a film coating layer to increase the roughness of the film layer, so that the components of the film layer are segregated, and finally the performance of the film layer is disordered.
The parameters of arc current and magnetic field voltage in the first step of film plating determine the performance of a Cr transition layer film, the Cr transition layer film needs to ensure good compactness, the parameters of arc current and magnetic field voltage are set too high to cause roughness increase, too low to cause compactness reduction, the bias voltage can ensure that the film layer has enough combination, and if the bias voltage is too low, the film layer has poor combination force, and if the bias voltage is too high to influence the roughness of the film layer;
in the second step of film coating, arc current and pulse magnetic field voltage are selected according to the evaporation characteristics of the multi-element target material elements and the characteristics of the arc target, the uniformity is improved when the magnetic field voltage is low, and the energy is increased and the uniformity is reduced when the magnetic field voltage is high; the direct current magnetic field voltage is used for regulating and controlling the segregation of the multicomponent components so as to obtain a compact composite membrane layer; the flow rate of the gas influences the evaporation of the target material and the compactness of the film; the bias voltage can ensure that the film layer has enough bonding property, if the bias voltage is too low, the bonding force of the film layer is poor, and if the bias voltage is too high, the roughness of the film layer can be influenced, and the growth stress of the film layer is increased; in the step, the frequency of the cathodic arc pulse magnetic field is increased, so that the density of critical atomic groups in unit area is improved, and a flat and uniform basic bottom film is obtained;
in the third step of film plating, the continuous growth of film crystal grains is blocked by an ion source and/or a magnetron sputtering source, the crystal grains do not have a specific preferential growth direction at the initial stage of film growth, and after the thickness of the film reaches a certain thickness value, the crystal grains grow along the specific direction, and a shielding phenomenon is generated along with the growth of the crystal grains, so that the compactness and the stability of the coating are reduced; according to the invention, the ion source and/or the magnetron sputtering source are/is used for injecting trace elements as incident particles in the deposition process of the film to continuously interrupt the growth of film grains and re-nucleation, so that the growth of the film grains is interfered and controlled to inhibit the increase of the growth stress of the film, an equiaxed crystal system is effectively formed, the compactness and stability of the coating are improved, the film hardness is improved, and the hardness can be improved by 21-33% compared with that of a conventional coating film; in addition, the power of the ion source and the magnetron sputtering source needs to be adjusted according to the property and the purpose of use, if the power is too low, the influence on the film growth is small, the increase of the coating hardness is small, and if the power is too high, although the increase of the hardness is large, the damage to the film tissue structure is possibly caused, and the stress is increased;
in the fourth step of film coating, arc current and magnetic field voltage are selected according to the evaporation characteristic of the AlTi target material and the characteristic of the arc target, and pulse magnetic field voltage, pulse frequency and direct current magnetic field voltage are all used for improving the compactness of a film layer in the fourth step; the flow rate of the gas influences the evaporation of the target material and the compactness of the film; the bias voltage can ensure that the film layer has enough combination property and hardness, and if the bias voltage is too low, the combination force of the film layer is poor, and if the bias voltage is too high, the hardness of the film layer can be influenced;
G. and (5) cooling.
Example 1
Taking the preparation of a surface coating of a high-speed steel or hard alloy cutter as an example, the preparation method comprises the following steps of:
(1) Pretreatment of
Before coating, the cutter is cleaned by adopting a conventional weak alkaline cleaning agent and absolute alcohol ultrasonic waves and then dried, and the cutter is placed in a coating chamber of coating equipment.
(2) Inspection coating equipment
Inflating the vacuum chamber and opening the oven door;
changing the target material and the window glass according to the requirement;
cleaning all parts of the furnace body by using a high-pressure air gun, wherein the pressure intensity of the high-pressure air gun is 0.6MPa;
selecting a proper clamp, loading a cutter to be coated, and confirming that the clamp is reliable in movement;
confirming the insulation condition of each evaporation source and the workpiece rotating frame, wherein the resistance value of each evaporation source and the workpiece rotating frame is more than 100KΩ;
closing the vapor deposition chamber and closing the air release valve.
(3) Vacuumizing and preheating
Starting a water chilling unit;
a rough pump and a pre-pumping valve are opened;
starting a compound vacuum gauge, opening a thermocouple gauge, and testing the vacuum of a foreline, wherein the vacuum is less than 5Pa;
starting a molecular pump, and closing a pre-pumping valve, opening a backing valve and a high vacuum valve when the molecular pump enters a normal working state and the vacuum degree of a vacuum chamber is less than 5Pa;
when the vacuum in the vacuum chamber is less than 0.1Pa, feeding Ar gas with the flow of 40sccm, and starting to heat to 400 ℃;
and opening the workpiece rotating frame, wherein the rotating speed is 1.5r/min.
(4) Glow cleaning
The pressure of the vacuum chamber is emphasized to 2.0Pa, and Ar gas with the flow of 120sccm is fed;
and starting a bias power supply, wherein the bias voltage is 900V, and the glow cleaning time is 5min.
(5) Vacuum-pumping
The bias power was turned off, the vacuum chamber was evacuated to 0.005Pa and the temperature was increased to 550 ℃.
(6) Ion source etching
Starting an ion source, wherein the power of the ion source is 3.0kw;
turning on a bias power supply, wherein the bias voltage is-350V;
feeding Ar gas with the flow rate of 40 sccm;
etching time is 60min.
(7) Coating film
Firstly plating a Cr layer: starting a row of Cr cathode evaporation sources, arc current 80A, pulse magnetic field voltage 0V, bias voltage direct current 80V and time 10min;
and then plating a multi-element nitride transition layer: two rows of corresponding cathode evaporation sources (AlCrSi evaporation sources, alCrW evaporation sources or AlTiCrSi evaporation sources) are started, and the control parameters are firstly adjusted as follows: arc current 90A, pulse magnetic field voltage 10V, pulse frequency 50.0Hz, direct current magnetic field voltage 0.5V, nitrogen flow 600sccm, bias voltage-50V to-100V, bias voltage increasing in the coating period, coating period 15min;
then plating a multi-element nitride layer: two rows of corresponding cathode evaporation sources (AlCrSi evaporation sources, alCrW evaporation sources or AlTiCrSi evaporation sources) are continuously started, and then the control parameters are adjusted as follows: arc current 80A, pulse magnetic field voltage 30V, pulse frequency 11.1Hz, direct current magnetic field voltage 1.5V, nitrogen flow 700sccm, bias voltage-100-50V, bias voltage decreasing in coating period, ion source power 0.5kw, coating period 240min;
finally, an AlTiN layer is plated, a row of AlTi cathode evaporation sources are started, the arc current is 90A, the pulse magnetic field voltage is 15V, the pulse frequency is 16.7Hz, the direct current magnetic field voltage is 1.0V, the nitrogen flow is 800sccm, the bias voltage is-50 to-100V, the bias voltage is increased gradually in the coating period, and the coating period is 30min;
(8) Cooling
Cooling for 120min after coating.
The performance of the cutter after film plating is detected, and as can be seen from the ball mark morphology graph shown in figure 1, the thickness of the thick film nitride coating of the cutter prepared by the process is 9.447 mu m, which is far beyond the thickness of the coating prepared by the traditional vacuum cathode arc ion plating technology; as can be seen from the hardness charts shown in FIGS. 2 to 4, the Vickers hardness of the base film of the Cr/AlTiCrSiN/AlTiN coating prepared by the process of the invention is 878-879 HV 25 The Vickers hardness of the intermediate layer is 2378-2387 HV 25 The Vickers hardness of the surface layer is 3637-3680 HV 25 The method comprises the steps of carrying out a first treatment on the surface of the As can be seen from the scratch test results shown in FIG. 5, the friction coefficient of the prepared Cr/AlCrWN/AlTiN coating is about 0.1, and the scratch bonding force LC 2 The coating is larger than 100N, can be improved by 30% compared with the conventional coating, has high hardness, low elastic modulus and effectively improves the plastic deformation resistance.
Example 2
By carrying out comparative experiments on cutters coated with different cutters under different processing object conditions, experimental data are as follows:
dry turning effect
Wet turning effect
From the data, the thickness of the thick film nitride coating is far higher than that of the traditional cutter, and when the cutter with the thick film nitride coating is used for carrying out different cutting operations, the cutting time of the cutter with the thick film nitride coating is obviously longer than that of the cutter with the traditional coating on the premise of consistent cutting speed, feeding amount and cutting depth, and the service life of the cutter with the thick film nitride coating is far longer than that of the cutter with the traditional coating, so that the service life of the cutter with the thick film nitride coating can be effectively prolonged.
Claims (2)
1. The preparation method of the thick film nitride coating of the cutter is characterized by comprising the following steps of: the thick film nitride coating of the cutter is a multi-element multi-layer coating formed by plating a Cr layer, a multi-element nitride layer and an AlTiN layer on the surface of the cutter from inside to outside in sequence, wherein the multi-element nitride layer is an AlCrSiN layer, an AlCrWN layer or an AlTiCrSiN layer; coating by adopting a vacuum cathode arc ion plating technology, and assisting by an ion source assisted deposition technology and/or a pulse magnetic field or a direct current magnetic field; firstly, evaporating a Cr target material in Ar atmosphere to form a Cr transition layer film on the surface of a cutter, and then, forming a Cr transition layer film on the surface of the cutter in N 2 Evaporating the multi-element compound target material under atmosphere to form multi-element nitride film with thickness of 7.5-10 μm, and finally forming the multi-element nitride film in N 2 Evaporating the AlTi target material in the atmosphere to form an AlTiN film;
the method comprises the following steps:
A. cleaning and drying the cutter;
B. vacuumizing the vacuum chamber and preheating to 400 ℃;
C. the pressure of the vacuum chamber is emphasized to 2.0Pa, ar gas with the flow of 120-240 sccm is fed, a bias power supply is started, the bias voltage is-500-1000V, and glow cleaning is carried out for 5-10 min;
D. closing a bias power supply, vacuumizing to 0.005Pa, and preheating to 550 ℃;
E. starting an ion source, wherein the power of the ion source is 1.0-3.0 kw, starting a bias power supply, the bias voltage is-300 to-400V, feeding Ar gas with the flow of 40-80 sccm, and etching for 40-60 min;
F. firstly, starting a Cr cathode evaporation source, an arc power supply 80-90A, a pulse magnetic field voltage 0V, a bias voltage direct current 80-100V, and a coating time 5-10 min; then starting the multi-compound cathode evaporation source, and firstly adjusting the control parameters as follows: arc current 80-90A, pulse magnetic field voltage 10-20V, pulse frequency 33.3-66.7 Hz, DC magnetic field voltage 0.5-2.0V, nitrogen flow 600-800 sccm, bias voltage-50-100V, bias voltage increasing in coating period, coating period 5-15 min; the control parameters are then adjusted as: arc current 80-90A, pulse magnetic field voltage 15-30V, pulse frequency 11.1-33.3 Hz, direct current magnetic field voltage 1.5-3.0V, nitrogen flow 600-800 sccm, bias voltage-100-50V, bias voltage decreasing in the coating period, starting ion source and/or sputtering source, ion source power 0.5-1.5 kw, sputtering source power 1-2 kw, coating time 180-360 min; finally, starting an AlTi cathode evaporation source, wherein the arc current is 80-100A, the pulse magnetic field voltage is 15-30V, the pulse frequency is 11.1-16.7 Hz, the direct current magnetic field voltage is 0.5-1.5V, the nitrogen flow is 500-700 sccm, the bias voltage is-50 to-130V, the bias voltage is increased gradually in the coating period, and the coating time is 20-40 min;
G. cooling for 120-150 min after coating.
2. A method of preparing a thick film nitride coating for a tool according to claim 1, wherein: the thickness of the Cr transition layer film is 100-200 nm; the AlTiN film has a thickness of 0.3 to 0.7 μm.
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| CN111349901A (en) * | 2020-03-27 | 2020-06-30 | 中国科学院力学研究所 | Preparation method of high-temperature-resistant alumina thick film coating for cutting tool |
| WO2021006739A1 (en) * | 2019-07-11 | 2021-01-14 | Knight Acquisition B.V. | Saw blade or other cutting tool comprising a coating |
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| CN107130213A (en) * | 2017-05-03 | 2017-09-05 | 成都真锐科技涂层技术有限公司 | Multicomponent alloy laminated film Preparation equipment and preparation method |
| CN107365963A (en) * | 2017-05-03 | 2017-11-21 | 四川大学 | PVD oxide coating preparation methods |
| CN108930021A (en) * | 2018-06-06 | 2018-12-04 | 广东工业大学 | A kind of nanometer multilayer AlTiN/AlTiVCuN coating and its preparation method and application |
| CN108796432A (en) * | 2018-09-12 | 2018-11-13 | 广东工业大学 | A kind of AlTiN coatings and preparation method thereof |
| WO2021006739A1 (en) * | 2019-07-11 | 2021-01-14 | Knight Acquisition B.V. | Saw blade or other cutting tool comprising a coating |
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