CN109161841B - AlCrN/AlCrSiN superhard nano composite multilayer coating and preparation method and application thereof - Google Patents

AlCrN/AlCrSiN superhard nano composite multilayer coating and preparation method and application thereof Download PDF

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CN109161841B
CN109161841B CN201810842580.7A CN201810842580A CN109161841B CN 109161841 B CN109161841 B CN 109161841B CN 201810842580 A CN201810842580 A CN 201810842580A CN 109161841 B CN109161841 B CN 109161841B
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alcrn
alcrsin
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composite multilayer
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CN109161841A (en
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王启民
钟星
吴正涛
许雨翔
伍一铭
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Guangdong University of Technology
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Guangdong University of Technology
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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
    • C23C14/0021—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

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  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
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  • Organic Chemistry (AREA)
  • Cutting Tools, Boring Holders, And Turrets (AREA)
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Abstract

The invention belongs to the technical field of cutter coating preparation, and discloses an AlCrN/AlCrSiN superhard nano composite multilayer coating as well as a preparation method and application thereof. The coating is prepared by adopting a pulse arc ion plating technology, and an AlCrN layer with the thickness of 0.2-1 mu m is deposited in the preparation process to be used as a transition layer between the coating and a substrate, so that a support is provided for a nano multilayer structure; the nanometer multilayer structure is realized through the rotation of the workpiece rotating frame; AlCrN intermediate layers and AlCrSiN intermediate layers are alternately deposited to form AlCrN/AlCrSiN nano composite multilayer functional layers, and the components of the AlCrN/AlCrSiN nano composite multilayer functional layers are Al: 18-32 at.%, Cr: 10-25 at.%, Si: 1-10 at.%, N: 45-57 at.%. The nano multilayer structure refines the size of columnar crystals, has good high hardness, high toughness, high wear resistance and high-temperature oxidation resistance, and is a cutter coating with good application prospect.

Description

AlCrN/AlCrSiN superhard nano composite multilayer coating and preparation method and application thereof
Technical Field
The invention belongs to the technical field of cutter coating preparation, and particularly relates to an AlCrN/AlCrSiN superhard nano composite multilayer coating as well as a preparation method and application thereof.
Background
Modern manufacturing industry developments are not free from cutting tools, placing higher and more demanding requirements on the tools. The environment-friendly, high-speed, high-precision and intelligent cutting is a pursuit target of cutting processing; materials with high strength, high hardness, high toughness, difficult cutting and the like are in a great variety, which has no small challenge on the cutter, while the hard alloy cutter coating has excellent performance on cutting processing under the new trend.
The AlCrN coating layer has excellent heat and high temperature resistance due to the formation of a stable alloy phase at high temperatures, and excellent mechanical properties such as high hardness, high wear resistance, and good chip removal ability, but has relatively high residual stress, which results in increased hardness and reduced adhesion. Whereas the AlCrSiN coating layer having a nanocomposite structure by doping Si has both nanocrystals having high hardness and Si having high heat resistance due to the presence of both3N4Amorphous and has excellent high-temperature characteristicsWhile having a lower residual stress. Through the design of a multilayer structure, the balance among the residual stress, the hardness and the fracture toughness is better, and the crack is prevented from being spread so as to be more controllable. The prepared AlCrN/AlCrSiN multilayer coating has the advantages of lower residual stress, high hardness, better wear resistance and high-temperature oxidation resistance, and is suitable for being applied in harsh processing working conditions.
The method for preparing the AlCrN/AlCrSiN nano composite multilayer cutter coating by using the pulse arc ion plating technology is not reported yet.
Disclosure of Invention
In order to overcome the defects in the prior art, the invention mainly aims to provide an AlCrN/AlCrSiN superhard nano composite multilayer coating; the coating has the characteristics of high hardness, high bonding strength, excellent high-temperature stability and wear resistance, and the deposited coating cutter is suitable for cutting and processing materials which are difficult to process under severe conditions.
The invention also aims to provide a preparation method of the AlCrN/AlCrSiN superhard nanocomposite multilayer coating, which adopts a pulse arc ion plating technology.
Still another object of the present invention is to provide an application of the above AlCrN/AlCrSiN superhard nanocomposite multilayer coating.
The purpose of the invention is realized by the following technical scheme:
an AlCrN/AlCrSiN superhard nano composite multilayer coating comprises a substrate, an AlCrN transition layer and an AlCrN/AlCrSiN nano composite multilayer functional layer from bottom to top; the AlCrN/AlCrSiN nano composite multilayer functional layer is formed by alternately depositing AlCrN intermediate layers and AlCrSiN intermediate layers with a modulation ratio of 1:1.5, and the modulation period is 10-35 nm; the AlCrN/AlCrSiN nano composite multilayer functional layer comprises the following elements in atomic percentage: 18-32 at.% of Al, 10-25 at.% of Cr, 1-10 at.% of Si, and 45-57 at.% of N.
The thickness of the AlCrN transition layer is 0.2-1 μm, and the thickness of the AlCrN/AlCrSiN nano composite multilayer functional layer is 2-8 μm.
The substrate base body is WC-Co hard alloy or a high-speed steel cutter.
The AlCrN/AlCrSiN superhard nanocomposite multilayer coating has a nanocomposite and nanocomposite multilayer structure, and when the modulation wavelength is in a nanoscale range, a superhard effect of abnormal hardness increase exists, the hardness is greater than 40GPa, and the AlCrN/AlCrSiN superhard nanocomposite multilayer coating belongs to a superhard coating.
The preparation method of the AlCrN/AlCrSiN superhard nano composite multilayer coating comprises the following operation steps:
(1) pre-treating a substrate, namely performing sand blasting and polishing treatment on the substrate, then performing ultrasonic cleaning for 10-30 min by using acetone and alcohol in sequence, then drying by using a drying furnace, then putting into a vacuum chamber, placing on a workpiece rotating stand, turning on a heater to heat the chamber to 300-500 ℃, and vacuumizing the vacuum chamber to the vacuum degree of 3-6 × 10-3Pa below;
(2) pulse etching: introducing Ar gas of 50-200 sccm and Kr gas of 50-100 sccm, setting the bias voltage of a workpiece rotating frame to be-650-1000V, setting the frequency to be 10-240 kHz, and performing pulse etching on the surface of the substrate for 10-20 min;
(3) d, direct current etching: introducing 100-300 sccm Ar gas and 50-100 sccm Kr gas, setting the bias voltage of a workpiece rotating stand to-150-300V, setting the ion source current to be 15-30A, and performing direct-current etching on the surface of the substrate for 20-50 min;
(4) depositing an AlCrN transition layer: adjusting the bias voltage of the workpiece rotating frame to-80 to-180V, and introducing N of 250 to 400sccm2Igniting an AlCr target, adjusting the air pressure to 1.0-3.0 Pa, adjusting the temperature of a vacuum chamber to 300-450 ℃, enabling the output current waveform of the pulse arc power supply to be rectangular wave or sawtooth wave, outputting pulse average current of 60-90A, and adjusting the frequency: 5-200 Hz, duty ratio: 1-70%, and depositing an AlCrN transition layer for 10-40 min;
(5) depositing AlCrN/AlCrSiN nano composite multilayer functional layer: adjusting the bias voltage of the workpiece rotating frame to-80 to-180V, and introducing N of 250 to 400sccm2And (2) adjusting the air pressure to 1-3 Pa, controlling the temperature of a vacuum chamber to 300-450 ℃, igniting an AlCr target and an AlCrSi target, wherein the waveform of the current output by the pulse arc power supply is rectangular wave or sawtooth wave, the average current of the output pulse is 60-90A, and the frequency is as follows: 5-200 Hz, duty ratio: 1-70% and deposition time is 1-4 h, and alternately depositing AlCrN on the AlCrN transition layer by revolving the workpiece frameThe interlayer and the AlCrSiN interlayer form an AlCrN/AlCrSiN nano composite multilayer functional layer;
(6) and after the deposition is finished, closing the power supply, opening the vacuum chamber to take out the sample after the temperature of the vacuum chamber is reduced to 100 ℃, and cooling to room temperature to form the AlCrN/AlCrSiN superhard nano composite multilayer coating.
In the steps (4) and (5), the atomic percentages of the elements of the AlCr target are Al: 50-70 at.%, Cr: 30-50 at.%; in the step (5), the atomic percentages of the elements of the AlCrSi target are Cr: 25-40 at.%, Al: 40-70 at.%, Si: 5 to 20 at.%.
In the step (5), the revolution speed of the workpiece frame is 1-5 r/min, the revolution drives the rotation, and the revolution rotation speed and the rotation speed are in a relation of 1: 3.
The AlCrN/AlCrSiN superhard nano composite multilayer coating is applied to the fields of cutter cutting and surface protection coatings.
Compared with the prior art, the invention has the following advantages and beneficial effects:
(1) compared with the traditional arc ion plating, the pulse arc ion plating has the advantages that the discharging process is pulse and discontinuous, stronger and higher-density plasma is generated, the average current is smaller, and the prepared coating has fewer large particles on the surface and more compact film tissue.
(2) The invention has better residual stress, hardness and fracture toughness through multilayer structure design, and can prevent crack from diffusing more controllably.
(3) The AlCrN/AlCrSiN multilayer coating cutter prepared by the method has better wear resistance and high-temperature oxidation resistance, is suitable for cutters applied in harsh machining working conditions, can meet the requirement of high-speed machining on better performance of cutter materials, and has huge market potential and use value.
Drawings
FIG. 1 is a schematic view of a pulsed arc deposition apparatus used in the present invention;
FIG. 2 is a cross-sectional profile of an AlCrN/AlCrSiN nanocomposite multilayer functional layer according to the present invention;
FIG. 3 is a nano indentation displacement load diagram of the AlCrN, AlCrSiN, AlCrN/AlCrSiN nano composite multilayer functional layer according to the present invention;
FIG. 4 is an XRD pattern of AlCrN, AlCrSiN, AlCrN/AlCrSiN nanocomposite multilayer functional layers of the present invention;
FIG. 5 is a cross-sectional profile and corresponding EDS line scan analysis of the AlCrN/AlCrSiN ultra hard nanocomposite multilayer coating of the present invention after oxidation at 1100 deg.C for 2 hours;
FIG. 6 is a friction curve plot of the AlCrN/AlCrSiN ultra hard nanocomposite multilayer coating of the present invention at RT, 600 deg.C and 800 deg.C.
Detailed Description
The present invention is further illustrated by the following examples, which are provided only for illustrating the present invention, but the scope of the present invention is not limited thereto.
In the following embodiment, a schematic diagram of alternately depositing an AlCrN/AlCrSiN superhard nano composite multilayer coating by adopting pulse arc ion plating is shown in FIG. 1, a workpiece rotating frame revolves to drive rotation in the process of depositing the coating, and when a sample faces a pulse arc AlCr target, a substrate deposits an AlCrN intermediate layer; when the AlCrSiN film is opposite to the AlCrY target, a layer of AlCrSiN intermediate layer is deposited; the AlCrN intermediate layer and the AlCrSiN intermediate layer are alternately deposited to form an AlCrN/AlCrSiN nano composite multilayer functional layer, and the rotating speed of the workpiece frame determines the thickness of each AlCrN layer and each AlCrSiN layer.
The atomic percentages of the elements of the AlCr target used in the examples were Al: 50-70 at.%, Cr: 30-50 at.%, and the atomic percentages of the elements of the AlCrSi target are Cr: 25-40 at.%, Al: 40-70 at.%, Si: 5 to 20 at.%.
Example 1
An AlCrN/AlCrSiN superhard nano composite multilayer coating comprises a substrate, an AlCrN transition layer and an AlCrN/AlCrSiN nano composite multilayer functional layer from bottom to top; the transition layer is attached to a WC-Co hard alloy or high-speed steel cutter substrate base body, and the thickness of the AlCrN coating is 0.2 mu m; the AlCrN/AlCrSiN nano composite multilayer functional layer is attached to the transition layer and has a thickness of 4 micrometers. The AlCrN/AlCrSiN nano composite multilayer functional layer comprises the following components: 29 at.%, Cr: 17 at.%, Si: 2 at.%, N: 52 at.%; the AlCrN/AlCrSiN nano composite multilayer functional layer is formed by alternately depositing AlCrN intermediate layers and AlCrSiN intermediate layers with a modulation ratio of 1:1.5, and the modulation period is 30-35 nm.
The preparation method of the AlCrN/AlCrSiN superhard nano composite multilayer coating adopts a pulse arc ion plating technology, and the preparation method of the coating comprises the following specific steps:
(1) pre-treating the substrate, sand blasting and polishing the substrate, ultrasonic cleaning with acetone and alcohol for 15min, baking in a baking oven, loading in a vacuum chamber, placing on a workpiece rotating stand, heating to 500 deg.C by turning on a heater, and vacuumizing to vacuum degree of 5.0 × 10-3Pa below;
(2) pulse etching: introducing Ar gas of 200sccm and Kr gas of 50sccm, setting the bias voltage of a workpiece rotating frame to be-1000V, setting the frequency to be 240kHz, and performing pulse etching on the surface of the substrate for 10 min;
(3) d, direct current etching: introducing 150sccm Ar gas and 80sccm Kr gas, setting the bias voltage of a workpiece rotating frame to be-300V, setting the current of an ion source to be 30A, and carrying out direct-current etching on the surface of the substrate for 30 min;
(4) depositing an AlCrN transition layer: the bias voltage of the workpiece rotating stand is adjusted to-100V, and N of 300sccm is introduced2Igniting an AlCr target, adjusting the air pressure to 1Pa, adjusting the temperature of the vacuum chamber to 400 ℃, enabling the output current waveform of the pulse arc power supply to be rectangular wave, outputting pulse average current 80A, and adjusting the frequency: 10Hz, duty cycle: 5%, depositing an AlCrN transition layer for 10 min;
(5) depositing AlCrN/AlCrSiN nano composite multilayer coating: setting the revolution speed of the workpiece rotating frame to be 1.5r/min, the revolution drives the rotation, the rotation speed is 4.5r/min, the bias voltage is adjusted to-100V, and introducing N of 300sccm2And gas, adjusting the gas pressure to 1Pa, adjusting the temperature of the vacuum chamber to 400 ℃, igniting an AlCr target and an AlCrSi target, wherein the output current waveform of the pulse arc power supply is pulse average current 80A output by rectangular waves, and the frequency is as follows: 10Hz, duty cycle: 5 percent, depositing for 2 hours, and alternately depositing an AlCrN intermediate layer and an AlCrSiN intermediate layer on the AlCrN transition layer through revolution of a workpiece frame to form an AlCrN/AlCrSiN nano composite multilayer functional layer; when the temperature of the vacuum chamber is reduced to below 100 ℃, beatingAnd opening the vacuum chamber, taking out the sample, and cooling to room temperature to form the AlCrN/AlCrSiN superhard nano composite multilayer coating.
FIG. 2 is a cross-sectional view of the AlCrN/AlCrSiN nanocomposite multilayer functional layer according to the embodiment of the present invention. As can be seen from FIG. 2, the coating has a compact structure and an obvious multi-layer structure, and the multi-layer structure can improve the mechanical property of the coating, prevent cracks from diffusing and improve the cutting performance of the coated cutter.
Example 2
An AlCrN/AlCrSiN superhard nano composite multilayer coating comprises a substrate, an AlCrN transition layer and an AlCrN/AlCrSiN nano composite multilayer functional layer from bottom to top; the transition layer is attached to a WC-Co hard alloy or high-speed steel cutter substrate base body, and the thickness of the AlCrN coating is 0.3 mu m; the AlCrN/AlCrSiN nano composite multilayer functional layer is attached to the transition layer and has a thickness of 3 micrometers. The AlCrN/AlCrSiN nano composite multilayer functional layer comprises the following components: 25 at.%, Cr: 18 at.%, Si: 3 at.%, N: 54 at.%; the AlCrN/AlCrSiN nano composite multilayer functional layer is formed by alternately depositing AlCrN intermediate layers and AlCrSiN intermediate layers with a modulation ratio of 1:1.5, and the modulation period is 27-32 nm.
The preparation method of the AlCrN/AlCrSiN superhard nano composite multilayer coating adopts a pulse arc ion plating technology, and the preparation method of the coating comprises the following specific steps:
(1) pre-treating the substrate, sand blasting and polishing the substrate, ultrasonic cleaning with acetone and alcohol for 15min, baking in a baking oven, loading in a vacuum chamber, placing on a workpiece rotating stand, heating to 450 deg.C by turning on a heater, and vacuumizing to vacuum degree of 5.0 × 10-3Pa below;
(2) pulse etching: introducing 150sccm Ar gas and 80sccm Kr gas, setting the bias voltage of the workpiece rotating frame to be-800V, the frequency to be 200kHz, and performing pulse etching on the surface of the substrate for 15 min;
(3) d, direct current etching: introducing 150sccm Ar gas and 100sccm Kr gas, setting the bias voltage of the workpiece rotating frame to-200V, setting the ion source current to be 25A, and performing direct-current etching on the surface of the substrate for 40 min.
(4) Depositing an AlCrN transition layer: the bias voltage of the workpiece rotating stand is adjusted to-120V, and N of 350sccm is introduced2Igniting an AlCr target, adjusting the air pressure to 1Pa, adjusting the temperature of the vacuum chamber to 400 ℃, enabling the output current waveform of the pulse arc power supply to be rectangular wave, outputting pulse average current 75A, and adjusting the frequency: 100Hz, duty cycle: 10 percent, depositing an AlCrN transition layer for 13 min;
(5) depositing AlCrN/AlCrSiN nano composite multilayer coating: setting the revolution speed of the workpiece rotating frame to be 2r/min, the revolution drives the rotation, the rotation speed is 6r/min, the bias voltage is adjusted to-120V, and introducing N of 350sccm2And gas, adjusting the gas pressure to 1Pa, adjusting the temperature of the vacuum chamber to 400 ℃, igniting an AlCr target and an AlCrSi target, wherein the output current waveform of the pulse arc power supply is pulse average current 75A output by rectangular waves, and the frequency is as follows: 100Hz, duty cycle: 10 percent, depositing for 1.5h, and alternately depositing an AlCrN intermediate layer and an AlCrSiN intermediate layer on the AlCrN transition layer through revolution of a workpiece frame to form an AlCrN/AlCrSiN nano composite multilayer functional layer; and opening the vacuum chamber when the temperature of the vacuum chamber is reduced to be below 100 ℃, taking out the sample, and cooling to room temperature to form the AlCrN/AlCrSiN superhard nano composite multilayer coating.
FIG. 3 is a nano indentation displacement load diagram of the AlCrN, AlCrSiN, AlCrN/AlCrSiN nano composite multilayer functional layer according to the present invention; the preparation process of the single AlCrN coating and the AlCrSiN coating is consistent with the preparation process of the multilayer AlCrN/AlCrSiN coating. It can be observed from fig. 3 that the compressive displacement of the AlCrN/AlCrSiN nanocomposite multilayer coating prepared by the embodiment of the present invention under the same load is smaller than that of the AlCrN coating and the AlCrSiN coating, and it is known that the hardness of the AlCrN/AlCrSiN nanocomposite multilayer coating prepared by the present invention is higher than that of the AlCrN and AlCrSiN single layer coating, and the hardness reaches more than 38 GPa.
Example 3
An AlCrN/AlCrSiN superhard nano composite multilayer coating comprises a substrate, an AlCrN transition layer and an AlCrN/AlCrSiN nano composite multilayer functional layer from bottom to top; the transition layer is attached to a WC-Co hard alloy or high-speed steel cutter substrate base body, and the thickness of the AlCrN coating is 0.4 mu m; the AlCrN/AlCrSiN nano composite multilayer functional layer is attached to the transition layer and has a thickness of 2 micrometers. The AlCrN/AlCrSiN nano composite multilayer functional layer comprises the following components: 23 at.%, Cr: 14 at.%, Si: 2 at.%, N: 56 at.%; the AlCrN/AlCrSiN nano composite multilayer functional layer is formed by alternately depositing AlCrN intermediate layers and AlCrSiN intermediate layers with a modulation ratio of 1:1.5, and the modulation period is 22-28 nm.
The preparation method of the AlCrN/AlCrSiN superhard nano composite multilayer coating adopts a pulse arc ion plating technology, and the preparation method of the coating comprises the following specific steps:
(1) pre-treating the substrate, sand blasting and polishing the substrate, ultrasonic cleaning with acetone and alcohol for 15min, baking in a baking oven, loading in a vacuum chamber, placing on a workpiece rotating stand, heating to 450 deg.C by turning on a heater, and vacuumizing to vacuum degree of 5.0 × 10-3Pa below;
(2) pulse etching: introducing 150sccm Ar gas and 80sccm Kr gas, setting the bias voltage of the workpiece rotating frame to be-800V, the frequency to be 200kHz, and performing pulse etching on the surface of the substrate for 15 min;
(3) d, direct current etching: introducing 150sccm Ar gas and 100sccm Kr gas, setting the bias voltage of the workpiece rotating frame to-200V, setting the ion source current to be 25A, and performing direct-current etching on the surface of the substrate for 40 min.
(4) Depositing an AlCrN transition layer: the bias voltage of the workpiece rotating stand is adjusted to-120V, and N of 350sccm is introduced2Igniting an AlCr target, adjusting the air pressure to 2Pa, adjusting the temperature of the vacuum chamber to 400 ℃, enabling the output current waveform of the pulse arc power supply to be rectangular wave, outputting pulse average current 75A, and adjusting the frequency: 100Hz, duty cycle: 10 percent, depositing an AlCrN transition layer for 20 min;
(5) depositing AlCrN/AlCrSiN nano composite multilayer coating: setting the revolution speed of the workpiece rotating frame to be 2r/min, the revolution drives the rotation, the rotation speed is 6r/min, the bias voltage is adjusted to-100V, and introducing N of 350sccm2And gas, adjusting the gas pressure to 1.5Pa, adjusting the temperature of the vacuum chamber to 400 ℃, igniting the AlCr target and the AlCrSi target, wherein the output current waveform of the pulse arc power supply is pulse average current 75A output by rectangular waves, and the frequency is as follows: 100Hz, duty cycle: 10 percent, the deposition time is 1.5h, and AlCrN intermediate layers and AlCrSiN intermediate layers are alternately deposited on the AlCrN transition layers through the revolution of a workpiece frame to form AlCrN/AlCrSiN nanoCompounding a plurality of functional layers; and opening the vacuum chamber when the temperature of the vacuum chamber is reduced to be below 100 ℃, taking out the sample, and cooling to room temperature to form the AlCrN/AlCrSiN superhard nano composite multilayer coating.
FIG. 4 is an XRD pattern of AlCrN, AlCrSiN, AlCrN/AlCrSiN nanocomposite multilayer functional layers of the present invention; the preparation process of the single AlCrN coating and the AlCrSiN coating is consistent with the preparation process of the multilayer AlCrN/AlCrSiN coating. As can be seen from fig. 4, the AlCrN, AlCrSiN coatings show mainly fcc-CrN in three orientations (111) (200) (220), while the AlCrN/AlCrSiN nanocomposite multilayer coatings show single-phase cubic and cubic wurtzite structures, respectively, indicating that the Si addition reduces the metastable dissolution limit of AlN in CrN. And for the discovery of Si3N4The diffraction peak of (A) indicates an amorphous structure, and the AlCrSiN nano composite structure can be speculated to be composed of amorphous Si3N4(Al, Cr) N wrapped with nanocrystalline; coherent strain and internal energy play a key role in coherent and incoherent growth of multilayer coatings, where the interfacial energy can be minimized by coherent growth through the templating effect.
Example 4
An AlCrN/AlCrSiN superhard nano composite multilayer coating comprises a substrate, an AlCrN transition layer and an AlCrN/AlCrSiN nano composite multilayer functional layer from bottom to top; the transition layer is attached to a WC-Co hard alloy or high-speed steel cutter substrate base body, and the thickness of the AlCrN coating is 0.25 mu m; the AlCrN/AlCrSiN nano composite multilayer functional layer is attached to the transition layer and has a thickness of 3 micrometers. The AlCrN/AlCrSiN nano composite multilayer functional layer comprises the following components: 24 at.%, Cr: 19 at.%, Si: 4 at.%, N: 53 at.%; the AlCrN/AlCrSiN nano composite multilayer functional layer is formed by alternately depositing AlCrN intermediate layers and AlCrSiN intermediate layers with a modulation ratio of 1:1.5, and the modulation period is 15-20 nm.
The preparation method of the AlCrN/AlCrSiN superhard nano composite multilayer coating adopts a pulse arc ion plating technology, and the preparation method of the coating comprises the following specific steps:
(1) pretreatment of a matrix: performing sand blasting and polishing treatment on a cutter substrate, then ultrasonically cleaning the cutter substrate for 15min by acetone and alcohol in sequence, and drying the cutter substrate by a drying furnaceLoading into vacuum chamber, placing on workpiece rotating stand, heating to 450 deg.C with heater, and vacuumizing to vacuum degree of 5.0 × 10-3Pa below;
(2) pulse etching: introducing 150sccm Ar gas and 80sccm Kr gas, setting the bias voltage of the workpiece rotating frame to be-800V, the frequency to be 200kHz, and performing pulse etching on the surface of the substrate for 15 min;
(3) d, direct current etching: introducing 150sccm Ar gas and 100sccm Kr gas, setting the bias voltage of the workpiece rotating frame to-200V, setting the ion source current to be 25A, and performing direct-current etching on the surface of the substrate for 40 min.
(4) Depositing an AlCrN transition layer: the bias voltage of the workpiece rotating stand is adjusted to-120V, and N of 350sccm is introduced2Igniting an AlCr target, adjusting the air pressure to 2Pa, adjusting the temperature of the vacuum chamber to 400 ℃, enabling the output current waveform of the pulse arc power supply to be rectangular wave, outputting pulse average current 70A, and adjusting the frequency: 10Hz, duty cycle: 5%, depositing an AlCrN transition layer for 20 min;
(5) depositing AlCrN/AlCrSiN nano composite multilayer coating: setting the revolution speed of the workpiece rotating frame to be 3r/min, the revolution drives the rotation, the rotation speed is 9r/min, the bias voltage is adjusted to-120V, and introducing N of 350sccm2And gas, adjusting the gas pressure to 2Pa, adjusting the temperature of the vacuum chamber to 400 ℃, igniting an AlCr target and an AlCrSi target, wherein the output current waveform of the pulse arc power supply is pulse average current 70A output by rectangular waves, and the frequency is as follows: 10Hz, duty cycle: 5 percent, depositing for 2 hours, and alternately depositing an AlCrN intermediate layer and an AlCrSiN intermediate layer on the AlCrN transition layer through revolution of a workpiece frame to form an AlCrN/AlCrSiN nano composite multilayer functional layer; and opening the vacuum chamber when the temperature of the vacuum chamber is reduced to be below 100 ℃, taking out the sample, and cooling to room temperature to form the AlCrN/AlCrSiN superhard nano composite multilayer coating.
FIG. 5 is the cross-sectional morphology and corresponding EDS line scan analysis of the AlCrN/AlCrSiN ultra hard nanocomposite multilayer coating of this example after oxidation at 1100 deg.C for 2 hours; as shown in FIG. 5, the thickness of the oxide layer after oxidation at 1100 ℃ for 2 hours was only about 0.7. mu.m, since dense (Al, Cr) was formed on the surface2O3And SiO2The oxide film blocks the oxygen from entering, so that the oxide film has excellent high-temperature oxidation performance.
Example 5
An AlCrN/AlCrSiN superhard nano composite multilayer coating comprises a substrate, an AlCrN transition layer and an AlCrN/AlCrSiN nano composite multilayer functional layer from bottom to top; the transition layer is attached to a WC-Co hard alloy or high-speed steel cutter substrate base body, and the thickness of the AlCrN coating is 0.6 mu m; the AlCrN/AlCrSiN nano composite multilayer functional layer is attached to the transition layer and has a thickness of 4 micrometers. The AlCrN/AlCrSiN nano composite multilayer functional layer comprises the following components: 23 at.%, Cr: 14 at.%, Si: 8 at.%, N: 55 at.%; the AlCrN/AlCrSiN nano composite multilayer functional layer is formed by alternately depositing AlCrN intermediate layers and AlCrSiN intermediate layers in a modulation ratio of 1:1.5, and the modulation period is 18-23 nm.
The preparation method of the AlCrN/AlCrSiN superhard nano composite multilayer coating adopts a pulse arc ion plating technology, and the preparation method of the coating comprises the following specific steps:
(1) pre-treating the substrate, sand blasting and polishing the substrate, ultrasonic cleaning with acetone and alcohol for 15min, baking in a baking oven, loading in a vacuum chamber, placing on a workpiece rotating stand, heating to 450 deg.C by turning on a heater, and vacuumizing to vacuum degree of 5.0 × 10-3Pa below;
(2) pulse etching: introducing 150sccm Ar gas and 80sccm Kr gas, setting the bias voltage of the workpiece rotating frame to be-800V, the frequency to be 200kHz, and performing pulse etching on the surface of the substrate for 15 min;
(3) d, direct current etching: introducing 150sccm Ar gas and 100sccm Kr gas, setting the bias voltage of the workpiece rotating frame to-200V, setting the ion source current to be 25A, and performing direct-current etching on the surface of the substrate for 40 min.
(4) Depositing an AlCrN transition layer: the bias voltage of the workpiece rotating stand is adjusted to-120V, and N of 350sccm is introduced2Igniting an AlCr target, adjusting the air pressure to 2Pa, adjusting the temperature of the vacuum chamber to 400 ℃, enabling the output current waveform of the pulse arc power supply to be rectangular wave, outputting pulse average current 70A, and adjusting the frequency: 50Hz, duty cycle: 10 percent, depositing an AlCrN transition layer for 30 min;
(5) depositing AlCrN/AlCrSiN nano composite multilayer coating: rotating the workpieceSetting revolution speed of the frame at 2.5r/min, rotating with revolution speed of 7.5r/min, adjusting bias voltage to-120V, introducing 350sccm N2And gas, adjusting the air pressure to 2Pa, adjusting the temperature of the vacuum chamber to 400 ℃, igniting an AlCr target and an AlCrSi target, wherein the output current waveform of the pulse arc power supply is pulse average current 80A output by rectangular waves, and the frequency is as follows: 50Hz, duty cycle: 10 percent, depositing for 2.5 hours, and alternately depositing an AlCrN intermediate layer and an AlCrSiN intermediate layer on the AlCrN transition layer through revolution of a workpiece frame to form an AlCrN/AlCrSiN nano composite multilayer functional layer; and opening the vacuum chamber when the temperature of the vacuum chamber is reduced to be below 100 ℃, taking out the sample, and cooling to room temperature to form the AlCrN/AlCrSiN superhard nano composite multilayer coating.
FIG. 6 is a graph of the friction curves of the AlCrN/AlCrSiN ultra hard nanocomposite multilayer coatings of this example at RT, 600 deg.C and 800 deg.C; as can be seen from fig. 6, as the friction temperature increases, the friction coefficient decreases; has a low friction coefficient at 800 ℃. Shows that the AlCrN/AlCrSiN coating has better wear-reducing and wear-resisting properties
Example 6
An AlCrN/AlCrSiN superhard nano composite multilayer coating comprises a substrate, an AlCrN transition layer and an AlCrN/AlCrSiN nano composite multilayer functional layer from bottom to top; the transition layer is attached to a WC-Co hard alloy or high-speed steel cutter substrate base body, and the thickness of the AlCrN coating is 0.5 mu m; the AlCrN/AlCrSiN nano composite multilayer functional layer is attached to the transition layer and is 5 micrometers thick. The AlCrN/AlCrSiN nano composite multilayer functional layer comprises the following components: 19 at.%, Cr: 22 at.%, Si: 8 at.%, N: 51 at.%; the AlCrN/AlCrSiN nano composite multilayer functional layer is formed by alternately depositing AlCrN intermediate layers and AlCrSiN intermediate layers with a modulation ratio of 1:1.5, and the modulation period is 10-15 nm.
The preparation method of the AlCrN/AlCrSiN superhard nano composite multilayer coating adopts a pulse arc ion plating technology, and the preparation method of the coating comprises the following specific steps:
(1) pretreatment of a matrix: carrying out sand blasting and polishing treatment on a cutter substrate, then carrying out ultrasonic cleaning for 15min by using acetone and alcohol in sequence, then drying by using a drying oven, then loading into a vacuum chamber, and placing on a workpiece rotating stand; turning on the heater will chamberHeating to 450 deg.C, and vacuumizing the vacuum chamber to vacuum degree of 5.0 × 10-3Pa below;
(2) pulse etching: introducing 150sccm Ar gas and 80sccm Kr gas, setting the bias voltage of the workpiece rotating frame to be-800V, the frequency to be 200kHz, and performing pulse etching on the surface of the substrate for 15 min;
(3) d, direct current etching: introducing 150sccm Ar gas and 100sccm Kr gas, setting the bias voltage of the workpiece rotating frame to-200V, setting the ion source current to be 25A, and performing direct-current etching on the surface of the substrate for 40 min.
(4) Depositing an AlCrN transition layer: the bias voltage of the workpiece rotating stand is adjusted to-150V, and N of 350sccm is introduced2Igniting an AlCr target, adjusting the air pressure to 3Pa, adjusting the temperature of a vacuum chamber to 350 ℃, wherein the output current waveform of the pulse arc power supply is rectangular wave, the output pulse average current is 60A, and the frequency is as follows: 200Hz, duty cycle: 3%, depositing an AlCrN transition layer for 40 min;
(5) depositing AlCrN/AlCrSiN nano composite multilayer coating: setting the revolution speed of the workpiece rotating frame to be 4r/min, the revolution drives the rotation, the rotation speed is 12r/min, the bias voltage is adjusted to-150V, and introducing N of 350sccm2And gas, adjusting the air pressure to 3Pa, adjusting the temperature of a vacuum chamber to 350 ℃, igniting an AlCr target and an AlCrSi target, wherein the output current waveform of the pulse arc power supply is pulse average current 60A output by rectangular waves, and the frequency is as follows: 200Hz, duty cycle: 3 percent, depositing for 3 hours, and alternately depositing an AlCrN intermediate layer and an AlCrSiN intermediate layer on the AlCrN transition layer through revolution of a workpiece frame to form an AlCrN/AlCrSiN nano composite multilayer functional layer; and opening the vacuum chamber when the temperature of the vacuum chamber is reduced to be below 100 ℃, taking out the sample, and cooling to room temperature to form the AlCrN/AlCrSiN superhard nano composite multilayer coating. The coating detection result shows that: the bonding force is more than 70N detected by a scratching method.
The above embodiments are preferred embodiments of the present invention, but the present invention is not limited to the above embodiments, and any other changes, modifications, substitutions, combinations, and simplifications which do not depart from the spirit and principle of the present invention should be construed as equivalents thereof, and all such changes, modifications, substitutions, combinations, and simplifications are intended to be included in the scope of the present invention.

Claims (5)

1. A preparation method of an AlCrN/AlCrSiN superhard nano composite multilayer coating is characterized by comprising the following operation steps:
(1) pre-treating a substrate, namely performing sand blasting and polishing treatment on the substrate, then performing ultrasonic cleaning for 10-30 min by using acetone and alcohol in sequence, then drying by using a drying furnace, then putting into a vacuum chamber, placing on a workpiece rotating stand, turning on a heater to heat the chamber to 300-500 ℃, and vacuumizing the vacuum chamber to the vacuum degree of 3-6 × 10-3Pa below;
(2) pulse etching: introducing Ar gas of 50-200 sccm and Kr gas of 50-100 sccm, setting the bias voltage of a workpiece rotating stand to be-650-1000V, the frequency to be 10-240 kHz, and performing pulse etching on the surface of the substrate for 10-20 min;
(3) d, direct current etching: introducing Ar gas of 100-300 sccm and Kr gas of 50-100 sccm, setting the bias voltage of a workpiece rotating stand to-150-300V, setting the ion source current to be 15-30A, and carrying out direct-current etching on the surface of the substrate for 20-50 min;
(4) depositing an AlCrN transition layer: adjusting the bias voltage of the workpiece rotating frame to-80 to-180V, and introducing N of 250 to 400sccm2Igniting an AlCr target, adjusting the air pressure to 1.0-3.0 Pa, adjusting the temperature of a vacuum chamber to 300-450 ℃, enabling the output current waveform of the pulse arc power supply to be rectangular wave or sawtooth wave, outputting pulse average current of 60-90A, and adjusting the frequency: 5-200 Hz, duty ratio: 1-70%, and depositing an AlCrN transition layer for 10-40 min;
(5) depositing AlCrN/AlCrSiN nano composite multilayer functional layer: adjusting the bias voltage of the workpiece rotating frame to-80 to-180V, and introducing N of 250 to 400sccm2And (2) adjusting the air pressure to 1-3 Pa, adjusting the temperature of the vacuum chamber to 300-450 ℃, igniting the AlCr target and the AlCrSi target, wherein the output current waveform of the pulse arc power supply is rectangular wave or sawtooth wave, the output pulse average current is 60-90A, and the frequency is as follows: 5-200 Hz, duty ratio: 1-70%, depositing for 1-4 h, and alternately depositing an AlCrN intermediate layer and an AlCrSiN intermediate layer on the AlCrN transition layer by revolving a workpiece frame to form an AlCrN/AlCrSiN nano composite multilayer functional layer;
(6) after the deposition is finished, the power supply is turned off, the vacuum chamber is opened to take out the sample after the temperature of the vacuum chamber is reduced to 100 ℃, and the sample is cooled to the room temperature to form the AlCrN/AlCrSiN superhard nano composite multilayer coating;
the coating comprises a substrate base body, an AlCrN transition layer and an AlCrN/AlCrSiN nano composite multilayer functional layer from bottom to top; the AlCrN/AlCrSiN nano composite multilayer functional layer is formed by alternately depositing AlCrN intermediate layers and AlCrSiN intermediate layers with a modulation ratio of 1:1.5, and the modulation period is 10-35 nm; the AlCrN/AlCrSiN nano composite multilayer functional layer comprises the following elements in atomic percentage: 18-32 at.% of Al, 10-25 at.% of Cr, 1-10 at.% of Si, and 45-57 at.% of N.
2. The method of claim 1, wherein: in the steps (4) and (5), the atomic percentages of the elements of the AlCr target are Al: 50-70 at.%, Cr: 30-50 at.%; and (5) the atomic percentages of the elements of the AlCrSi target are Cr: 25-40 at.%, Al: 40-70 at.%, Si: 5 to 20 at.%.
3. The method of claim 1, wherein: in the step (5), the revolution speed of the workpiece frame is 1-5 r/min, the revolution drives the rotation, and the revolution rotation speed and the rotation speed are in a relation of 1: 3.
4. The method of claim 1, wherein: the thickness of the AlCrN transition layer is 0.2-1 μm, and the thickness of the AlCrN/AlCrSiN nano composite multilayer functional layer is 2-8 μm.
5. The method of claim 1, wherein: the substrate base body is WC-Co hard alloy or a high-speed steel cutter.
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