CN110578123A - High-hardness AlTiN/AlTiSiN multilayer nano composite coating and preparation process thereof - Google Patents
High-hardness AlTiN/AlTiSiN multilayer nano composite coating and preparation process thereof Download PDFInfo
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- 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
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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
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- C23C14/024—Deposition of sublayers, e.g. to promote adhesion of the coating
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- 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
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- 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
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Abstract
The invention discloses a high-hardness AlTiN/AlTiSiN multilayer nano composite coating and a preparation process thereof, and belongs to the technical field of composite coating preparation. The AlTiN/AlTiSiN multilayer nano composite coating is formed by alternately overlapping AlTiN layers and AlTiSiN layers, the modulation period of the coating is 150-1000nm, and the period number is not less than 2. The composite coating is prepared by adopting an arc ion coating technology, and the process is as follows: selecting a metal Ti target, an AlTi target and an AlTiSi target, depositing a TiN transition layer after glow cleaning and bombardment cleaning, finally introducing nitrogen as reaction gas, and alternately starting the AlTi target and the AlTiSi target according to a set modulation period to deposit the composite coating. The coating prepared by the invention has compact tissue structure, strong binding force between the coating and the substrate, higher hardness and strength and good wear resistance.
Description
Technical Field
The invention relates to the technical field of composite coating preparation, in particular to a high-hardness AlTiN/AlTiSiN multilayer nano composite coating and a preparation process thereof.
Background
in recent years, the use of wear resistant hard coatings on mechanical, forging and forming devices has become increasingly important, not only to save costs, but also to improve the service life of the material. The AlTiN coating is widely applied to high-speed steel and hard alloy cutters at present due to the excellent high-temperature hardness and oxidation resistance, which is attributed to the increase of aluminum element to a great extent. Compared with a binary coating TiN, the AlTiN coating is used as a protective layer of the cutter, and can reduce the abrasion loss and the fracture caused by impact. Although the oxidation resistance of the AlTiN coating is obviously improved compared with other binary coatings, the requirements of high hardness, high toughness, wear resistance and the like under certain high-speed cutting or dry cutting environments cannot be met.
in order to develop a multilayer nano composite coating with compact structure, high hardness and wear resistance, the patent adopts the arc ion coating technology to deposit the AlTiN/AlTiSiN multilayer nano composite coating on a metal or alloy matrix, thereby further improving the mechanical property of the single-layer coating and realizing the service life and excellent performance of the multilayer coating.
Disclosure of Invention
The invention aims to provide a high-hardness AlTiN/AlTiSiN multilayer nano composite coating and a preparation process thereof.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows:
a high-hardness AlTiN/AlTiSiN multilayer nano composite coating is deposited on a metal or hard alloy substrate, and is formed by alternately stacking AlTiN layers and AlTiSiN layers, wherein the modulation period of the coating is 150-1000nm, and the periodicity is more than or equal to 2.
The modulation ratio of the AlTiN layer to the AlTiSiN layer is 1:1, the total thickness of the deposited coating is 3 μm.
The AlTiN/AlTiSiN multilayer nano composite coating is of a face-centered cubic structure, no low-hardness hexagonal phase is generated, and the preferred orientation crystal face of the coating is a diffraction peak of (Ti, Al) N (200).
The hardness of the AlTiN/AlTiSiN multilayer nano composite coating is more than 28GPa, and the bonding force with a base material is more than 100N.
The preparation process of the high-hardness AlTiN/AlTiSiN multilayer nano composite coating is characterized in that an AlTiN/AlTiSiN multilayer nano composite coating is deposited on a substrate by adopting an arc ion coating technology, and a target material is selected from a pure metal Ti target, an AlTi alloy target and an AlTiSi alloy target (the target material purity is 99.9 wt%); when depositing the AlTiN/AlTiSiN multilayer nano composite coating, the Ti target is firstly started, then the AlTi target and the AlTiSi target are alternately started to deposit the corresponding AlTiN layer and AlTiSiN layer, and the deposition pressure, the gas flow and the arc flow parameters of each target when depositing the AlTiN layer and the AlTiSiN layer are controlled, so that the AlTiN/AlTiSiN multilayer nano composite coating with the AlTiN layer and the AlTiSiN layer alternately superposed with each other is prepared on the substrate.
When depositing the AlTiN/AlTiSiN multilayer nano composite coating, arc flows are set to be 40-100A; when an AlTi target is started to deposit an AlTiN coating, setting a bias voltage of 60-150V (duty ratio of 50% -90%), and introducing argon and nitrogen to adjust the deposition pressure to 0.5-2 Pa; when an AlTiSi target is started to deposit an AlTiSiN coating, setting a bias voltage of 80-100V (duty ratio of 50% -90%), and introducing argon and nitrogen to adjust the deposition pressure to 1-3 Pa; different modulation periods and deposition times of the coating are set according to the desired thickness of the coating.
When depositing the AlTiN coating, the flow of the introduced argon is 50sccm, the flow of the introduced nitrogen is 350sccm, and the total flow is 400 sccm; when the AlTiSiN coating is deposited, the flow rate of argon is 50sccm, the flow rate of nitrogen is 600sccm, and the total flow rate is 650 sccm.
The preparation process of the high-hardness AlTiN/AlTiSiN multilayer nano composite coating specifically comprises the following steps:
(1) The targets are uniformly distributed around the vacuum chamber of the arc ion plating equipment so as to ensure that the furnace cavity has higher plasma concentration in the deposition process; placing the pretreated substrate on a central rotating frame of a coating chamber; the vacuum chamber is pumped to 3 × 10 by mechanical pump and molecular pump-3Pa below;
(2) Glow bombardment cleaning: firstly, glow washing the substrate for 10-30 min by adopting high negative bias glow, starting a Ti target after glow washing, and adjusting the bias to-800V, -600V, -400V and-200V in sequence to respectively carry out bombardment washing on the surface of the substrate for 2 min;
(3) And (3) depositing a TiN transition layer: depositing a TiN transition layer with the thickness of 10-350 nm on the surface of the substrate after glow bombardment cleaning so as to improve the binding force between the coating and the substrate;
(4) Depositing a multi-layer composite coating: and starting the alloy AlTi target and the AlTiSi target to deposit the multilayer composite coating.
In the step (2), the glow cleaning process includes: heating the furnace chamber to 200-500 ℃, introducing argon gas of 200-400 sccm, setting pulse bias voltage of-600-1000V, and performing glow cleaning on the substrate;
in the step (2), the bombardment cleaning process is as follows: after glow cleaning, starting the Ti target, adjusting the argon flow to be 50-100 sccm, and cleaning for 2min under negative bias conditions of-800V, -600V, -400V and-200V respectively.
In the step (3), the process of depositing the TiN transition layer is as follows: after glow bombardment cleaning, setting a bias voltage of 50-100V (duty ratio of 60% -90%), starting the Ti target, introducing argon gas flow of 50sccm and nitrogen gas flow of 200sccm, adjusting the deposition pressure to 0.5-1.2 Pa, and depositing a transition layer TiN for 10-30 min.
The design mechanism of the invention is as follows:
The invention adds Si element in the AlTiN coating and utilizes the solid solution strengthening effect of Al and Ti elements and amorphous Si3N4The grain is refined, the hardness is improved, and the AlTiN coating and the AlTiSiN are alternately arranged to form a multilayer nano composite coating, so that the AlTiN/AlTiSiN multilayer composite coating has excellent characteristics obviously superior to a single-layer coating and meets the wide requirements of people in the field of wear-resistant materials.
The nano multilayer film prepared by the invention is a modulation structure, namely a structure with a certain repetition period. Two different coatings are alternately deposited in a nanoscale size, the obtained multilayer nano composite structure has a superhard phenomenon that the hardness is abnormally increased, the advantages of different materials are integrated, the defects of a single-layer film are overcome, and compared with the single-layer film, the multilayer nano composite structure has better comprehensive mechanical properties, particularly high hardness, high toughness and excellent wear resistance.
the invention has the following advantages:
1. The AlTiN/AlTiSiN multilayer nano composite coating developed by the invention has higher hardness and toughness, low friction coefficient and good wear resistance.
2. the nano composite AlTiN/AlTiSiN coating developed by the invention has higher high-temperature thermal stability and corrosion resistance, and can be used in the field of high-speed dry cutting processing.
3. The AlTiN/AlTiSiN nano composite coating developed by the invention has uniform thickness and compact structure, and has good bonding strength with a matrix.
4. The AlTiN/AlTiSiN nano composite coating prepared by the invention has good repeatability of the preparation process, wide application range and very strong practicability.
Drawings
FIG. 1 is a diffraction pattern of AlTiN/AlTiSiN nano composite coating prepared by arc ion plating technology.
FIG. 2 is a surface topography of the AlTiN/AlTiSiN nano composite coating prepared by the arc ion plating technique.
FIG. 3 is a cross-sectional view of the AlTiN/AlTiSiN nano composite coating prepared by the arc ion plating technique.
FIG. 4 is a nano-indentation curve diagram of the AlTiN/AlTiSiN nano-composite coating prepared by the arc ion plating technology.
FIG. 5 is a graph of the morphology of AlTiN/AlTiSiN nanocomposite coatings prepared by arc ion plating after scratch test.
FIG. 6 is a graph of a friction coefficient test for an AlTiN/AlTiSiN coating prepared using an arc ion plating technique.
Detailed Description
The present invention will be described in further detail by way of examples.
example 1
this example is a polished 304 stainless steel sheet with a 25X 30X 1mm sample size deposited with a multi-layer nanocomposite coating of AlTiN/AlTiSiN.
The substrate is pretreated firstly: ultrasonic cleaning in acetone and alcohol for 15 min, blowing with high purity nitrogen gas, and setting in sample rack inside vacuum chamber.
the coating process is carried out on an AIP-650 type arc ion coating machine, pure metal Ti targets, alloy AlTi targets and alloy AlTiSi targets (the purity is 99.9 wt.%) with the diameters of 100mm are used as target materials, and high-purity argon and nitrogen are respectively used as working gas and reaction gas.
the targets are uniformly distributed on the inner wall of the furnace body of the arc ion plating equipment so as to ensure that the furnace cavity has higher plasma concentration in the deposition process; placing the pretreated substrate on a central rotating frame of a coating chamber;
the vacuum chamber is pumped to 3 × 10 by mechanical pump and molecular pump-3And (3) turning on a heating system below Pa, raising the temperature to 430 ℃, introducing argon gas into a vacuum chamber to 400sccm, and setting the bias voltage to-800V to perform glow discharge cleaning on the surface of the sample for 20 min.
Then starting the Ti target, adjusting the argon flow to be 50-100 sccm, and adjusting negative bias to be-800V, -600V, -400V and-200V in sequence to respectively carry out bombardment cleaning for 2 minutes;
setting the bias voltage as 100V (duty ratio 60%), starting the Ti target, introducing 50sccm argon and 200sccm nitrogen, adjusting the deposition pressure to be 0.8Pa, and depositing the transition layer TiN for 20 min;
Finally, alternately starting the AlTi target and the AlTiSi target, wherein the arc flow is set to be 80A; when the AlTi target is started to deposit each AlTiN layer: setting a bias voltage of 80V (duty ratio of 80%), introducing argon with the flow rate of 50sccm and nitrogen with the flow rate of 350sccm, and adjusting the deposition pressure to be 1 Pa; when starting an AlTiSi target to deposit each AlTiSiN layer, setting a bias voltage of 100V (duty ratio of 80%), introducing argon gas with the flow rate of 50sccm and nitrogen gas with the flow rate of 600sccm, adjusting the deposition pressure to be 2.8Pa, setting the modulation period of the coating to be 750nm, depositing 4 periods (total 8 layers), wherein the modulation ratio of the two coatings is 1:1, and the total thickness of the deposited coating is 3 microns.
Fig. 1 is a diffraction spectrum of the AlTiN/AlTiSiN nano composite coating prepared in this example, and it can be seen that the coating is composed of a coating with a face-centered cubic structure, no hexagonal phase with low hardness is generated, and the preferred orientation crystal plane of the coating is a diffraction peak of (Ti, Al) N (200).
FIG. 2 is a surface topography of a nanocomposite coating, which is characterized by a typical arc ion plating coating, having a dense and uniform texture, with a small amount of large particles on the surface.
FIG. 3 is a cross-sectional profile of a nanocomposite coating having a thickness of about 3 μm that bonds well to a substrate.
Fig. 4 is a graph of hardness value change of the nanocomposite coating tested using the nanoindentation technique. With the pressing of the nanoindentation probe, the hardness value of the test coating is rapidly increased to reach a plateau value, and then the hardness is gradually reduced due to the substrate effect. The plateau value is generally taken as the average hardness value of the coating. As can be seen, the hardness of the nanocomposite coating of this example was about 29 GPa.
Fig. 5 is a graph of scratch topography variation of the nanocomposite coating tested using the scratch tester. As can be seen from the figure, the coating has good bonding force, which reaches 102N.
FIG. 6 is a graph of the friction profile of the nanocomposite coating tested using a high temperature friction machine. The friction curve fluctuates due to the structure of the layers or due to the unevenness of the surface of the coating.
example 2
In this example, a multilayer nano composite coating of AlTiN/AlTiSiN was deposited on a polished cemented carbide substrate, and the sample size was 25X 30X 3 mm.
the substrate is pretreated firstly: ultrasonic cleaning in acetone and alcohol for 15 mm, blowing with high purity nitrogen, and setting in sample rack in vacuum chamber.
The coating process is carried out on an AIP-650 type arc ion coating machine, the target material adopts a pure metal Ti target, an alloy AlTi target and an AlTiSi alloy target (the purity is wt.99.9%) with the diameter of 100mm as the target material, and the working gas and the reaction gas respectively adopt high-purity argon and nitrogen.
All the targets are uniformly placed around the vacuum chamber of the arc ion plating equipment so as to ensure that the furnace cavity has higher plasma concentration in the deposition process; placing the pretreated substrate on a central rotating frame of a coating chamber;
The background of the vacuum chamber is firstly pumped to 3 multiplied by 10 by adopting a mechanical pump and a molecular pump-3Pa or less, turning on heatingThe temperature of the system is raised to 430 ℃, then argon gas is introduced into a vacuum chamber at 400sccm, and the bias voltage is set to-800V to carry out glow discharge cleaning on the surface of the sample for 20 min.
Then starting the Ti target, adjusting the argon flow to be 50-100 sccm, and adjusting negative bias to be-800V, -600V, -400V and-200V in sequence to respectively carry out bombardment cleaning for 2 minutes;
Setting the bias voltage as 100V (duty ratio 60%), starting the Ti target, introducing 50sccm argon and 200sccm nitrogen, adjusting the deposition pressure to be 0.8Pa, and depositing the transition layer TiN for 20 min;
finally, alternately starting the AlTi target and the AlTiSi target, wherein the arc flow is set to be 80A; when the AlTi target is started to deposit each AlTiN layer: setting a bias voltage of 80V (duty ratio of 80%), introducing argon with the flow rate of 50sccm and nitrogen with the flow rate of 350sccm, and introducing the argon and the nitrogen to adjust the deposition pressure to be 1 Pa; when starting the AlTiSi target to deposit each AlTiSiN layer, setting a bias voltage of 100V (duty ratio of 80%), introducing argon gas with the flow rate of 50sccm and nitrogen gas with the flow rate of 600sccm, introducing the argon gas and the nitrogen gas to adjust the deposition pressure to be 2.8Pa, setting the modulation period of the coating to be 375nm, setting the modulation ratio of the two coatings to be 1:1, and setting the total thickness of the deposited coating to be 3 μm.
The nanocomposite coating prepared in this example had the same phase composition and texture as the coating in example 1, and consisted of a coating of face centered cubic structure. The total thickness of the coating is about 3 mu m, and the hardness is as high as 32 Gpa.
Claims (10)
1. The high-hardness AlTiN/AlTiSiN multilayer nano composite coating is characterized in that: the coating is deposited on a metal or hard alloy matrix, the AlTiN/AlTiSiN multilayer nano composite coating is formed by alternately overlapping AlTiN layers and AlTiSiN layers, the modulation period of the coating is 150-1000nm, and the periodicity is more than or equal to 2.
2. The high hardness AlTiN/AlTiSiN multilayer nanocomposite coating of claim 1, wherein: the modulation ratio of the AlTiN layer to the AlTiSiN layer is 1:1, the total thickness of the deposited coating is 3 μm.
3. The high hardness AlTiN/AlTiSiN multilayer nanocomposite coating of claim 1, wherein: the AlTiN/AlTiSiN multilayer nano composite coating is of a face-centered cubic structure, no low-hardness hexagonal phase is generated, and the preferred orientation crystal face of the coating is a diffraction peak of (Ti, Al) N (200).
4. The high hardness AlTiN/AlTiSiN multilayer nanocomposite coating of claim 1, wherein: the hardness of the AlTiN/AlTiSiN multilayer nano composite coating is more than 28GPa, and the bonding force with a base material is more than 100N.
5. The process for preparing high-hardness AlTiN/AlTiSiN multilayer nano composite coating according to any one of claims 1 to 4, wherein: the process is characterized in that an AlTiN/AlTiSiN multilayer nano composite coating is deposited on a substrate by adopting an arc ion coating technology, and a target material is selected from a pure metal Ti target, an AlTi alloy target and an AlTiSi alloy target (the target material purity is 99.9 wt%); when depositing the AlTiN/AlTiSiN multilayer nano composite coating, the Ti target is firstly started, then the AlTi target and the AlTiSi target are alternately started to deposit the corresponding AlTiN layer and AlTiSiN layer, and the deposition pressure, the gas flow and the arc flow parameters of each target when depositing the AlTiN layer and the AlTiSiN layer are controlled, so that the AlTiN/AlTiSiN multilayer nano composite coating with the AlTiN layer and the AlTiSiN layer alternately superposed with each other is prepared on the substrate.
6. The preparation process of the high-hardness AlTiN/AlTiSiN multilayer nano composite coating according to claim 5, characterized in that: when depositing the AlTiN/AlTiSiN multilayer nano composite coating, setting arc flow to be 40-100A; when an AlTi target is started to deposit an AlTiN coating, setting a bias voltage of 60-150V (duty ratio of 50% -90%), and introducing argon and nitrogen to adjust the deposition pressure to 0.5-2 Pa; when an AlTiSi target is started to deposit an AlTiSiN coating, setting a bias voltage of 80-100V (duty ratio of 50% -90%), and introducing argon and nitrogen to adjust the deposition pressure to 1-3 Pa; different modulation periods and deposition times of the coating are set according to the desired thickness of the coating.
7. The preparation process of the high-hardness AlTiN/AlTiSiN multilayer nano composite coating according to claim 6, characterized in that: when depositing the AlTiN coating, the flow of the introduced argon is 50sccm, the flow of the introduced nitrogen is 350sccm, and the total flow is 400 sccm; when the AlTiSiN coating is deposited, the flow rate of argon is 50sccm, the flow rate of nitrogen is 600sccm, and the total flow rate is 650 sccm.
8. The process for preparing high-hardness AlTiN/AlTiSiN multilayer nano composite coating according to claim 7, characterized in that: the process specifically comprises the following steps:
(1) Placing the pretreated substrate on a central rotating stand of a coating chamber, and controlling the air pressure of the vacuum chamber to be 3 x 10-3pa below;
(2) Glow bombardment cleaning: firstly, glow washing the substrate for 10-30 min by adopting high negative bias glow, starting a Ti target after glow washing, and adjusting the bias to-800V, -600V, -400V and-200V in sequence to respectively carry out bombardment washing on the surface of the substrate for 2 min;
(3) And (3) depositing a TiN transition layer: depositing a TiN transition layer with the thickness of 10-350 nm on the surface of the substrate after glow bombardment cleaning so as to improve the binding force between the coating and the substrate;
(4) Depositing a multi-layer composite coating: and starting the alloy AlTi target and the AlTiSi target to deposit the multilayer composite coating.
9. The process for preparing high-hardness AlTiN/AlTiSiN multilayer nano composite coating according to claim 8, wherein: in the step (2), the glow cleaning process comprises the following steps: heating the furnace chamber to 200-500 ℃, introducing argon gas of 200-400 sccm, setting pulse bias voltage of-600-1000V, and performing glow cleaning on the substrate; the bombardment cleaning process comprises the following steps: after glow cleaning, starting the Ti target, adjusting the argon flow to be 50-100 sccm, and cleaning for 2min under negative bias conditions of-800V, -600V, -400V and-200V respectively.
10. The process for preparing high-hardness AlTiN/AlTiSiN multilayer nano composite coating according to claim 8, wherein: in the step (3), the process of depositing the TiN transition layer comprises the following steps: after glow bombardment cleaning, setting a bias voltage of 50-100V (duty ratio of 60% -90%), starting the Ti target, introducing argon gas flow of 50sccm and nitrogen gas flow of 200sccm, adjusting the deposition pressure to 0.5-1.2 Pa, and depositing a transition layer TiN for 10-30 min.
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| CN115948711A (en) * | 2022-12-14 | 2023-04-11 | 株洲华锐精密工具股份有限公司 | Composite hard coating and preparation method and application thereof |
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| CN114457304A (en) * | 2022-01-11 | 2022-05-10 | 厦门钨业股份有限公司 | TiAlMeN-TiAlN nano multilayer structure coating and preparation method and application thereof |
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Application publication date: 20191217 |