CN111155064A - Method for preparing TiAlSiN composite coating by high-power pulse magnetron sputtering - Google Patents
Method for preparing TiAlSiN composite coating by high-power pulse magnetron sputtering Download PDFInfo
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- C—CHEMISTRY; METALLURGY
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- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/34—Sputtering
- C23C14/35—Sputtering by application of a magnetic field, e.g. magnetron sputtering
- C23C14/352—Sputtering by application of a magnetic field, e.g. magnetron sputtering using more than one target
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- C23C14/0036—Reactive sputtering
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- 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
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- 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
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- 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
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Abstract
The invention discloses a method for preparing a TiAlSiN composite coating by high-power pulse magnetron sputtering, which comprises the following steps: s1, preparing: on HCVAC HCSH650 equipment, Ti target, TiAl alloy target and Si target are used as target materials, and the target material purity of each target is more than or equal to 99%; the Ti target and the TiAl target are connected with a high-power pulse magnetron sputtering power supply, and the Si target is connected with a radio frequency power supply; the revolution speed of the revolving frame hung with the high-speed steel or hard alloy cutter is 3-15 r/min, and the target base distance is 60-150 mm; respectively selecting high-purity Ar and high-purity N2 as working gas and reaction gas; s2, depositing a coating: the method comprises the following steps of 1, cleaning; 2. heating; 3. adjusting the pressure intensity; 4. glow cleaning; 5. bombarding and activating pure Ti; 6. depositing a Ti transition layer; 7. depositing a TiN transition layer; 8. depositing TIALN with high Ti content; 9. depositing TiAlN; 10. TIALSiN is deposited. The method has the advantages of controllable Si content, high deposition rate, composite structure formed by wrapping the nanocrystalline nitride by Si3N4, and excellent performance.
Description
Technical Field
The invention relates to a preparation method of a nano composite coating, in particular to a method for preparing a high-hardness and high-strength TiAlSiN nano composite coating by adopting a high-power pulse and radio frequency co-sputtering technology
Background
The cutter material mainly comprises high-speed steel and hard alloy. The high-speed steel has better toughness, but has low hardness, is very easy to tip when processing high-temperature alloy, has short service life and low efficiency; the hard alloy has better hardness, wear resistance and the like, and is the most commonly used material for cutting the high-temperature alloy. The coating technology can ensure that the cutter obtains excellent comprehensive mechanical properties, effectively improves the service life of the cutting cutter, the cutting efficiency and the quality of the processed surface, and greatly improves the machining efficiency. TiAlN is a common cutter coating, and Si element is doped into TiAlN to enhance the hardness and the wear resistance of the coating, thereby prolonging the service life.
The high-power pulse magnetron sputtering is a physical vapor deposition method which is newly developed and widely focused, obtains high metal ionization rate by utilizing higher pulse peak power (about 2-3 orders of magnitude of the traditional magnetron sputtering), and has remarkable technical advantages in the aspects of obtaining excellent film/base bonding force, controlling the microstructure of a coating, reducing the internal stress of the coating and the like. Compared with the traditional magnetron sputtering structure, the coating structure prepared by the high-power pulse technology is more compact, and the crystal grains are finer, so that the coating structure shows excellent comprehensive performance.
The radio frequency sputtering is that a radio frequency power supply is indirectly connected with two poles, electrons in oscillation motion obtain enough energy from a high-frequency electric field, and the electrons collide with gas molecules more effectively to generate higher ionization rate, so that higher deposition rate can be obtained under low pressure, and the prepared film is compact, high in purity, firm in adhesion with a substrate and good in process repeatability.
The slow deposition rate is an important reason for restricting the practical application of preparing the TiAlSiN coating by high-power pulse magnetron sputtering. Researchers adopt a technology of combining direct current magnetron sputtering and high-power pulse magnetron sputtering to improve the deposition rate of the TiAlSiN film, but the magnetron sputtering has a low ionization rate (< 10%), has the defects of non-compact film layer and poor film-substrate combination, weakens the advantages of the HIPIMS, deposits the film layer under high pressure, and reduces the energy reaching the surface of the substrate due to collision of sputtered particles and gas, so that the film layer becomes sparse and has poor performance. In addition, the published work mostly adopts AlSi or TiAlSi alloy targets, and the adjustment of the Si content ratio is inconvenient.
Disclosure of Invention
The invention aims to solve the technical problem of providing a method for preparing a TiAlSiN composite coating by high-power pulse magnetron sputtering3N4The wrapped composite structure has excellent performance.
The technical scheme adopted by the invention is as follows:
a method for preparing a TiAlSiN composite coating by high-power pulse magnetron sputtering is characterized by comprising the following steps:
s1, preparation
On HCVAC HCSH650 equipment (an experimental machine can be popularized to other equipment), Ti targets, TiAl alloy targets and Si targets are used as targets, and the target purity of each target is more than or equal to 99%; the Ti target and the TiAl target are connected with a high-power pulse magnetron sputtering power supply, and the Si target is connected with a radio frequency power supply; the revolution speed of the rotating frame hung with the high-speed steel or hard alloy cutter is 3-15 r/min, and the target-to-substrate distance (the distance between the target material and the substrate) is 60-150 mm; high-purity Ar and high-purity N2 (the purity is more than or equal to 99.9 percent) are respectively selected as the working gas and the reaction gas.
S2, depositing the coating
1. Cleaning: cleaning and drying a high-speed steel or hard alloy matrix in an ultrasonic cleaning machine, fixing the high-speed steel or hard alloy matrix on a rotating frame, and closing a furnace door; a vacuum unit consisting of a mechanical pump, a roots pump and a molecular pump is adopted for vacuumizing to more than 5.0 multiplied by 10 < -3 > Pa;
2. heating: when the vacuum of the furnace chamber is equal to or better than 5 multiplied by 10 < -3 > Pa, a heating system is started to heat the furnace chamber to 100-450 ℃;
3. adjusting the pressure: opening an Ar gas flow valve, and adjusting a throttle valve to enable the pressure of the furnace chamber to be 0.6-3 Pa;
4. glow cleaning: negative bias voltage of-600V to-1200V is applied to the high-speed steel or hard alloy cutter, the duty ratio is 30% -90%, and glow cleaning is carried out for 10-30 min;
5. bombardment activation of pure Ti: starting the Ti target material, wherein the power is 1-20KW, the peak current is 200-800A, the pulse time is 50-1000 mus, the pulse frequency is 50-500Hz, the negative bias is-300 to-600V, the duty ratio is 30% -90%, and the bombardment activation is carried out for 5-30 min;
6. and (3) depositing a Ti transition layer: regulating Ar gas flow, keeping the pressure intensity of a furnace chamber at 0.1-1Pa, reducing negative bias to-10 to-250V, depositing a pure Ti metal transition layer on the surface of a high-speed steel or hard alloy cutter for 30-60 min, wherein the power of a Ti target material is 1-20KW, the peak current is 200-800A, the pulse time is 50-1000 mu s, and the pulse frequency is 50-500Hz, so that the binding force between the coating and a substrate is improved;
7. and (3) depositing a TiN transition layer: simultaneously introducing N2 and Ar, wherein the flow of Ar is 30-100 sccm, adjusting nitrogen to ensure that the pressure of the vacuum chamber is 0.1-1Pa, the power of the Ti target is 1-20KW, the peak current is 200-800A, the pulse time is 50-1000 mus, and the pulse frequency is 50-500Hz, and depositing a TiN transition layer; the deposition time is 20-60 min;
8. deposition of high Ti content TIALN: simultaneously starting the Ti target and the TiAl target, wherein the target power is 1-20KW, the peak current is 200-800A, the pulse time is 50-1000 mus, the pulse frequency is 50-500Hz, and the TiAlN coating is deposited for 60-360 min;
9. deposition of TiAlN: keeping other parameters unchanged, closing the Ti target, and depositing the TiAlN coating for 120-360 min;
10. deposition of TIALSin: starting a radio frequency Si target with the power of 100-; and depositing a TiAlSiN coating on the surface of the high-speed steel or hard alloy substrate for 120-360 min.
And after the deposition is finished, closing the target power supply, the gas flow valve and the heater power supply, and taking out the coating when the temperature in the furnace is lower than 80 ℃.
The TiAlSiN nano composite coating can be applied to various metals and hard alloy substrates.
The invention has the advantages that:
1) the TiAlSiN composite coating developed by the invention adopts a coating obtained by a high-power pulse magnetron sputtering technology and a radio frequency co-sputtering technology, the deposition rate is high, and the content of Si in the coating is easy to control by adjusting process parameters.
2) The TiAlSiN composite coating developed by the invention adopts a high-power pulse magnetron sputtering technology and a radio frequency co-sputtering technology to obtain a coating with fine grains and compact structure.
3) The TiAlSiN composite coating developed by the invention has good high-temperature thermal stability and corrosion resistance, and can be used in the fields of high-speed high-precision cutting and dry cutting processing.
4) The TiAlSiN composite coating developed by the invention adopts high-power pulse magnetron sputtering and radio frequency co-sputtering technologies, has good bonding strength with a substrate, and has the advantages of simple preparation process, good repeatability, wide application range and very strong practicability.
Description of the drawings:
FIG. 1 is a layout diagram of a magnetic control cathode of a TiAlSiN composite coating device prepared by a high-power pulse and radio frequency co-sputtering technology;
FIG. 2 is a structural diagram of a TiAlSiN composite coating prepared by high-power pulse and radio-frequency co-sputtering technology.
Reference numerals in the figures refer to: 1. high speed steel or carbide cutters; 2. high power pulsed magnetron sputtering-titanium; 3. high power pulsed magnetron sputtering-titanium nitride; 4. high power pulse magnetron sputtering-titanium aluminum nitrogen; 5. high-power pulse magnetron sputtering and radio frequency magnetron sputtering-titanium aluminum silicon nitrogen.
Detailed Description
The present invention is further illustrated by the following examples.
Example 1
In this embodiment, a high power pulse and rf co-sputtering technique is used to prepare a TiAlSiN composite coating on a polished cemented carbide test piece, where the size of the cemented carbide test piece is 16 × 16 × 5 mm.
S1, preparation
On HCVAC HCSH650 equipment (an experimental machine can be popularized to other equipment), a Ti target, a TiAl alloy target (the alloy ratio is 1: 1) and a Si target are used as targets, and the target purity of each target is more than or equal to 99 percent; the Ti target and the TiAl target are connected with a high-power pulse magnetron sputtering power supply, and the Si target is connected with a radio frequency power supply; the revolution speed of the revolving frame hung with the high-speed steel or hard alloy cutter is 3r/min, and the target base distance (the distance between the target material and the base body) is 100 mm; high-purity Ar and high-purity N2 (the purity is more than or equal to 99.9%) are respectively selected as the working gas and the reaction gas.
S1, depositing
1. Cleaning: cleaning and drying a high-speed steel or hard alloy matrix in an ultrasonic cleaning machine, fixing the high-speed steel or hard alloy matrix on a rotating frame, and closing a furnace door; a vacuum unit consisting of a mechanical pump, a roots pump and a molecular pump is adopted for vacuumizing to more than 5.0 multiplied by 10 < -3 > Pa;
2. heating: when the vacuum of the furnace chamber is better than 5 multiplied by 10 < -3 > Pa, a heating system is started to heat the furnace chamber to 400 ℃;
3. adjusting the pressure: opening an Ar gas flow valve, and adjusting a throttle valve to enable the pressure of the furnace chamber to be 1 Pa;
4. glow cleaning: negative bias of-800V is added to the high-speed steel or hard alloy cutter, the duty ratio is 70%, and glow cleaning is carried out for 30 min;
5. bombardment activation of pure Ti: starting the Ti target material, wherein the power is 1KW, the peak current is 300A, the pulse time is 100 mus, the pulse frequency is 200Hz, the negative bias is-600V, the duty ratio is 70%, and the bombardment activation is carried out for 10 min;
6. and (3) depositing a Ti transition layer: regulating Ar gas flow, keeping the pressure of a furnace chamber at 0.5Pa, reducing negative bias to-250V, changing the power of the Ti target material to 5KW, the peak current to 300A, the pulse time to 100 mus and the pulse frequency to 200Hz, depositing a pure Ti metal transition layer on the surface of the high-speed steel or hard alloy cutter for 30min, and improving the binding force between the coating and the substrate;
7. and (3) depositing a TiN transition layer: simultaneously introducing N2 and Ar, wherein the flow of Ar is 100sccm, adjusting nitrogen to ensure that the pressure of the vacuum chamber is 0.4Pa, the power of the Ti target is 5KW, the peak current is 300A, the pulse time is 100 mus, and the pulse frequency is 200Hz, and depositing a TiN transition layer; the deposition time was 30 min.
8. Deposition of high Ti content TIALN: simultaneously starting the Ti target and the TiAl target, wherein the target power is 5KW, the peak current is 500A, the pulse time is 100 mu s, the pulse frequency is 200Hz, and the TiAlN coating is deposited for 60 min;
9. deposition of TiAlN: keeping other parameters unchanged, closing the Ti target, and depositing the TiAlN coating for 120 min;
10. deposition of TIALSin: starting a radio frequency Si target with the power of 500W; and depositing a TiAlSiN coating on the surface of the high-speed steel or hard alloy substrate for 240 min.
After the deposition is finished, the power supply of the target material, the gas flow valve and the heater are closed, and the coating is taken out when the temperature in the furnace is lower than 80 DEG C
According to the experimental result, the Si content in the obtained coating is 7%, the hardness of the obtained coating is 3550HV, the deposition rate is 2.1 mu m/h, and when a CNC (computerized numerical control) holed turning tool coated with the coating is used for carrying out cutting test on Cr40, the chip removal state is continuous and non-colored, which shows that the coating is high in hardness and good in cutting performance.
Example 2
The apparatus, process and process parameters were the same as in example 1 except that the RF Si target was turned on in step 10 at a power of 1100 w.
According to the experimental result, the Si content of the obtained coating is 9%, the coating hardness is 3847HV, the deposition rate is 2.3 mu m/h, and when a CNC (computerized numerical control) porous turning tool coated with the coating is used for carrying out cutting test on Cr40, the chip removal state is continuous and non-colored, which indicates that the coating hardness is high, the coating is not damaged in the cutting process, and the coating has an ideal chip removal state.
Example 3
The apparatus, process and process parameters were the same as in example 1 except that the RF Si target was turned on at 1700w in step 10.
According to the experimental measurement result, the content of Si in the obtained coating is 11%, the coating hardness is 3910HV, the deposition rate is 2.7 mu m/h, and when a CNC (computerized numerical control) holed turning tool coated with the coating is used for carrying out cutting test on Cr40, iron chips are not colored continuously, which indicates that the cutting performance of the coated cutting tool is excellent.
Example 4
In the embodiment, a TiAlSiN composite coating is prepared on a polished high-speed steel sheet by adopting a high-power pulse and radio frequency co-sputtering technology, and the size of a high-speed steel sample is D14 multiplied by 5 mm.
S1, preparation
On HCVAC HCSH650 equipment (an experimental machine can be popularized to other equipment), a Ti target, a TiAl alloy target (the alloy ratio is 1: 1) and a Si target are used as targets, and the target purity of each target is more than or equal to 99 percent; the Ti target and the TiAl target are connected with a high-power pulse magnetron sputtering power supply, and the Si target is connected with a radio frequency power supply; the revolution speed of the revolving frame hung with the high-speed steel or hard alloy cutter is 5r/min, and the target base distance (the distance between the target material and the base body) is 80 mm; high-purity Ar and high-purity N2 (the purity is more than or equal to 99.9%) are respectively selected as the working gas and the reaction gas.
S1, depositing
1. Cleaning: cleaning and drying a high-speed steel or hard alloy matrix in an ultrasonic cleaning machine, fixing the high-speed steel or hard alloy matrix on a rotating frame, and closing a furnace door; a vacuum unit consisting of a mechanical pump, a roots pump and a molecular pump is adopted for vacuumizing to more than 5.0 multiplied by 10 < -3 > Pa;
2. heating: when the vacuum of the furnace chamber is better than 5 multiplied by 10 < -3 > Pa, a heating system is started to heat the furnace chamber to 300 ℃;
3. adjusting the pressure: opening an Ar gas flow valve, and adjusting a throttle valve to enable the pressure of the furnace chamber to be 1 Pa;
4. glow cleaning: negative bias voltage of-700V is added to the high-speed steel or hard alloy cutter, the duty ratio is 70%, and glow cleaning is carried out for 30 min;
5. bombardment activation of pure Ti: starting the Ti target material, wherein the power is 1KW, the peak current is 400A, the pulse time is 100 mus, the pulse frequency is 200Hz, the negative bias is-600V, the duty ratio is 70%, and the bombardment activation is carried out for 10 min;
6. and (3) depositing a Ti transition layer: regulating Ar gas flow, keeping the pressure of a furnace chamber at 0.5Pa, reducing negative bias to-200V, changing the power of the Ti target material to 1KW, the peak current to 300A, the pulse time to 100 mus and the pulse frequency to 200Hz, depositing a pure Ti metal transition layer on the surface of the high-speed steel or hard alloy cutter for 30min, and improving the binding force between the coating and the substrate;
7. and (3) depositing a TiN transition layer: keeping the bias voltage at-200V, simultaneously introducing N2 and Ar, controlling the flow of Ar to be 100sccm, adjusting the nitrogen to ensure that the pressure of a vacuum chamber is 0.4Pa, the power of the Ti target is 5KW, the peak current is 300A, the pulse time is 100 mus, the pulse frequency is 200Hz, and depositing a TiN transition layer; the deposition time was 30 min.
8. Deposition of high Ti content TIALN: simultaneously starting the Ti target and the TiAl target, wherein the target power is 5KW, the peak current is 500A, the pulse time is 100 mu s, the pulse frequency is 200Hz, and the TiAlN coating is deposited for 60 min;
9. deposition of TiAlN: keeping other parameters unchanged, closing the Ti target, and depositing the TiAlN coating for 120 min;
10. deposition of TIALSin: starting a radio frequency Si target with the power of 800W; and depositing a TiAlSiN coating on the surface of the high-speed steel or hard alloy substrate for 240 min.
And after the deposition is finished, closing the target power supply, the gas flow valve and the heater power supply, and taking out the coating when the temperature in the furnace is lower than 80 ℃.
According to the experimental result, the hardness of the obtained coating is 3100HV, the deposition rate reaches 2.5 mu m/h, and when a CNC (computerized numerical control) porous turning tool coated with the coating is used for carrying out cutting test on Cr40, the chip removal state is continuous and non-colored, which indicates that the coating has high hardness and good cutting performance.
Example 5
In this embodiment, a high power pulse and rf co-sputtering technique is used to prepare a TiAlSiN composite coating on a polished cemented carbide test piece, where the size of the cemented carbide test piece is 16 × 16 × 5 mm.
S1, preparation
On HCVAC HCSH650 equipment (an experimental machine can be popularized to other equipment), Ti targets, TiAl alloy targets and Si targets are used as targets, and the target purity of each target is more than or equal to 99%; the Ti target and the TiAl target are connected with a high-power pulse magnetron sputtering power supply, and the Si target is connected with a radio frequency power supply; the revolution speed of the revolving frame hung with the high-speed steel or hard alloy cutter is 3r/min, and the target base distance (the distance between the target material and the base body) is 60 mm; high-purity Ar and high-purity N2 (the purity is more than or equal to 99.9 percent) are respectively selected as the working gas and the reaction gas.
S2, depositing the coating
1. Cleaning: cleaning and drying a high-speed steel or hard alloy matrix in an ultrasonic cleaning machine, fixing the high-speed steel or hard alloy matrix on a rotating frame, and closing a furnace door; a vacuum unit consisting of a mechanical pump, a roots pump and a molecular pump is adopted for vacuumizing to more than 5.0 multiplied by 10 < -3 > Pa;
2. heating: when the vacuum of the furnace chamber is better than 5 multiplied by 10 < -3 > Pa, a heating system is started to heat the furnace chamber to 100 ℃;
3. adjusting the pressure: opening an Ar gas flow valve, and adjusting a throttle valve to enable the pressure of the furnace chamber to be 0.6 Pa;
4. glow cleaning: applying negative bias of-600% to the high-speed steel or hard alloy tool, and glow cleaning at the duty ratio of 30% for 10 min;
5. bombardment activation of pure Ti: starting the Ti target material, wherein the power is 1KW, the peak current is 200A, the pulse time is 50 mus, the pulse frequency is 50Hz, the negative bias is-300, the duty ratio is 30%, and bombarding and activating are carried out for 5 min;
6. and (3) depositing a Ti transition layer: regulating Ar gas flow, keeping the pressure of a furnace chamber at 0.1Pa, reducing negative bias to-10V, depositing a pure Ti metal transition layer on the surface of a high-speed steel or hard alloy cutter for 30min, wherein the power of the Ti target is 1KW, the peak current is 200A, the pulse time is 50 mus, and the pulse frequency is 50Hz, so that the binding force between the coating and the substrate is improved;
7. and (3) depositing a TiN transition layer: simultaneously introducing N2 and Ar, wherein the flow rate of Ar is 30sccm, adjusting nitrogen to ensure that the pressure of a vacuum chamber is 0.1Pa, the power of the Ti target is 1KW, the peak current is 200A, the pulse time is 50 mus, and the pulse frequency is 50Hz, and depositing a TiN transition layer; the deposition time was 20 min.
8. Deposition of high Ti content TIALN: simultaneously starting the Ti target and the TiAl target, wherein the target power is 1KW, the peak current is 200A, the pulse time is 50 mu s, the pulse frequency is 50Hz, and the TiAlN coating is deposited for 60 min;
9. deposition of TiAlN: keeping other parameters unchanged, closing the Ti target, and depositing the TiAlN coating for 120 min;
10. deposition of TIALSin: turning on a radio frequency Si target with the power of 100 w; and depositing a TiAlSiN coating on the surface of the high-speed steel or hard alloy substrate for 120 min.
And after the deposition is finished, closing the target power supply, the gas flow valve and the heater power supply, and taking out the coating when the temperature in the furnace is lower than 80 ℃.
According to the experimental result, the hardness of the obtained coating is 3207HV, the deposition rate is 2 mu m/h, and when a CNC (computerized numerical control) porous turning tool coated with the coating is used for carrying out cutting test on Cr40, the chip removal state is continuous and non-colored, which indicates that the coating has high hardness and good cutting performance.
Example 6
In this embodiment, a high power pulse and rf co-sputtering technique is used to prepare a TiAlSiN composite coating on a polished cemented carbide test piece, where the size of the cemented carbide test piece is 16 × 16 × 5 mm.
S1, preparation
On HCVAC HCSH650 equipment (an experimental machine can be popularized to other equipment), Ti targets, TiAl alloy targets and Si targets are used as targets, and the target purity of each target is more than or equal to 99%; the Ti target and the TiAl target are connected with a high-power pulse magnetron sputtering power supply, and the Si target is connected with a radio frequency power supply; the revolution speed of the revolving frame hung with the high-speed steel or hard alloy cutter is 15r/min, and the target base distance (the distance between the target material and the base body) is 150 mm; high-purity Ar and high-purity N2 (the purity is more than or equal to 99.9 percent) are respectively selected as the working gas and the reaction gas.
S2, depositing the coating
1. Cleaning: cleaning and drying a high-speed steel or hard alloy matrix in an ultrasonic cleaning machine, fixing the high-speed steel or hard alloy matrix on a rotating frame, and closing a furnace door; a vacuum unit consisting of a mechanical pump, a roots pump and a molecular pump is adopted for vacuumizing to more than 5.0 multiplied by 10 < -3 > Pa;
2. heating: when the vacuum of the furnace chamber is better than 5 multiplied by 10 < -3 > Pa, a heating system is started to heat the furnace chamber to 450 ℃;
3. adjusting the pressure: opening an Ar gas flow valve, and adjusting a throttle valve to enable the pressure of the furnace chamber to be 3 Pa;
4. glow cleaning: negative bias of-1200V is applied to the high-speed steel or hard alloy cutter, and the cleaning is performed in glow with a duty ratio of 90% for 30 min;
5. bombardment activation of pure Ti: starting the Ti target material, wherein the power is 20KW, the peak current is 800A, the pulse time is 1000 mus, the pulse frequency is 500Hz, the negative bias is-600V, the duty ratio is 90 percent, and the bombardment activation is carried out for 30 min;
6. and (3) depositing a Ti transition layer: regulating Ar gas flow, keeping the pressure of a furnace chamber at 1Pa, reducing negative bias to-250V, depositing a pure Ti metal transition layer on the surface of a high-speed steel or hard alloy cutter for 60min, wherein the power of the Ti target is 20KW, the peak current is 800A, the pulse time is 1000 mus, and the pulse frequency is 500Hz, and improving the binding force between the coating and the substrate;
7. and (3) depositing a TiN transition layer: simultaneously introducing N2 and Ar, wherein the flow of Ar is 100sccm, adjusting nitrogen to ensure that the pressure of the vacuum chamber is 1Pa, the power of the Ti target is 20KW, the peak current is 800A, the pulse time is 1000 mus, and the pulse frequency is 500Hz, and depositing a TiN transition layer; deposition time 60min
8. Deposition of high Ti content TIALN: simultaneously starting the Ti target and the TiAl target, wherein the target power is 20KW, the peak current is 800A, the pulse time is 1000 mus, the pulse frequency is 500Hz, and the TiAlN coating is deposited for 360 min;
9. deposition of TiAlN: keeping other parameters unchanged, closing the Ti target, and depositing the TiAlN coating for 360 min;
10. deposition of TIALSin: starting a radio frequency Si target with power of 3000 w; and depositing a TiAlSiN coating on the surface of the high-speed steel or hard alloy substrate for 360 min.
And after the deposition is finished, closing the target power supply, the gas flow valve and the heater power supply, and taking out the coating when the temperature in the furnace is lower than 80 ℃.
According to the experimental result, the hardness of the obtained coating is 3600HV, the deposition rate is 2.8 mu m/h, and when a CNC (computerized numerical control) porous turning tool coated with the coating is used for carrying out cutting test on Cr40, the chip removal state is continuous and non-colored, which indicates that the coating is high in hardness and good in cutting performance.
Claims (5)
1. A method for preparing a TiAlSiN composite coating by high-power pulse magnetron sputtering is characterized by comprising the following steps:
s1, preparation
On vacuum plating equipment, a Ti target, a TiAl alloy target and a Si target are used as targets, and the purity of the target of each target is more than or equal to 99 percent; the Ti target and the TiAl target are connected with a high-power pulse magnetron sputtering power supply, and the Si target is connected with a radio frequency power supply; the revolution speed of the revolving frame hung with the high-speed steel or hard alloy cutter is 3-15 r/min, and the target base distance is 60-150 mm; the working gas and the reaction gas respectively adopt high-purity Ar and N2 with the purity of more than or equal to 99.9 percent;
s2, depositing the coating
Comprising the substeps of 10: deposition of TIALSin: starting a radio frequency Si target with the power of 100-; and depositing a TiAlSiN coating on the surface of the high-speed steel or hard alloy substrate for 120-360 min.
2. The method for preparing the TiAlSiN composite coating by the high-power pulse magnetron sputtering method according to claim 1, which is characterized in that: before the substep 10, the method further comprises a substep 9: deposition of TiAlN: keeping other parameters unchanged, closing the Ti target, and depositing the TiAlN coating for 120-360 min.
3. The method for preparing the TiAlSiN composite coating by the high-power pulse magnetron sputtering method according to claim 2, which is characterized in that: before substep 9, substep 8 is further included: deposition of high Ti content TIALN: and simultaneously starting the Ti target and the TiAl target, wherein the target power is 1-20KW, the peak current is 200-800A, the pulse time is 50-1000 mus, the pulse frequency is 50-500Hz, and the TiAlN coating is deposited for 60-360 min.
4. The method for preparing the TiAlSiN composite coating by the high-power pulse magnetron sputtering method according to claim 3, which is characterized in that: before the substep 8, the method further comprises a substep 7: and (3) depositing a TiN transition layer: simultaneously introducing N2 and Ar, wherein the flow of Ar is 30-100 sccm, adjusting nitrogen to ensure that the pressure of the vacuum chamber is 0.1-1Pa, the power of the Ti target is 1-20KW, the peak current is 200-800A, the pulse time is 50-1000 mus, and the pulse frequency is 50-500Hz, and depositing a TiN transition layer; the deposition time is 20-60 min.
5. The method for preparing the TiAlSiN composite coating by the high-power pulse magnetron sputtering method according to claim 4, which is characterized in that: before the substep 7, substeps 1-6 are also included:
1. cleaning: cleaning and drying a high-speed steel or hard alloy matrix in an ultrasonic cleaning machine, fixing the high-speed steel or hard alloy matrix on a rotating frame, and closing a furnace door; a vacuum unit consisting of a mechanical pump, a roots pump and a molecular pump is adopted for vacuumizing to more than 5.0 multiplied by 10 < -3 > Pa;
2. heating: when the vacuum of the furnace chamber is equal to or better than 5 multiplied by 10 < -3 > Pa, a heating system is started to heat the furnace chamber to 100-450 ℃;
3. adjusting the pressure: opening an Ar gas flow valve, and adjusting a throttle valve to enable the pressure of the furnace chamber to be 0.6-3 Pa;
4. glow cleaning: negative bias voltage of-600V to-1200V is applied to the high-speed steel or hard alloy cutter, the duty ratio is 30% -90%, and glow cleaning is carried out for 10-30 min;
5. bombardment activation of pure Ti: starting the Ti target material, wherein the power is 1-20KW, the peak current is 200-800A, the pulse time is 50-1000 mus, the pulse frequency is 50-500Hz, the negative bias is-300 to-600V, the duty ratio is 30% -90%, and the bombardment activation is carried out for 5-30 min;
6. and (3) depositing a Ti transition layer: regulating Ar gas flow, keeping the pressure intensity of the furnace chamber at 0.1-1Pa, reducing the negative bias to-10 to-250V, depositing a pure Ti metal transition layer on the surface of the high-speed steel or hard alloy cutter for 30-60 min, wherein the power of the Ti target material is 1-20KW, the peak current is 200-800A, the pulse time is 50-1000 mu s, and the pulse frequency is 50-500 Hz.
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| CN111945118A (en) * | 2020-09-10 | 2020-11-17 | 中国航发沈阳黎明航空发动机有限责任公司 | Preparation method of erosion-resistant reinforced coating of titanium alloy compressor blade |
| CN112575290A (en) * | 2020-11-23 | 2021-03-30 | 东莞市普拉提纳米科技有限公司 | Method for coating CBN cutter material |
| CN114107905A (en) * | 2021-11-08 | 2022-03-01 | 广州今泰科技股份有限公司 | Impact-resistant high-hardness coating and preparation method and application thereof |
| CN114147227A (en) * | 2021-12-10 | 2022-03-08 | 哈尔滨理工大学 | Bionic cutter based on bamboo fiber cell wall annular multi-wall-layer structure and preparation method thereof |
| CN114147227B (en) * | 2021-12-10 | 2022-10-11 | 哈尔滨理工大学 | Bionic cutter based on bamboo fiber cell wall annular multi-wall-layer structure and preparation method thereof |
| CN115216742A (en) * | 2022-07-14 | 2022-10-21 | 山东大学 | Hard alloy cutter gradient coating and preparation method thereof |
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