CN110257772B - AlTiSiCON superhard coating and preparation method thereof - Google Patents
AlTiSiCON superhard coating and preparation method thereof Download PDFInfo
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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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- C23C14/00—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
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Abstract
The invention relates to the field of vacuum coating, and provides an AlTiSiCN superhard coating, which is of a multilayer structure and sequentially comprises a TiN priming layer, an AlTiN layer, an AlTiSiCN layer and an AlTiSiCN surface layer from inside to outside; the AlTiN layer, the AlTiSiCN layer, the AlTiN layer and the AlTiSiCN layer between the TiN priming layer and the AlTiSiCN surface layer form an AlTiN and AlTiSiCN staggered layer. The invention also provides a method for preparing the AlTiSiCON superhard coating by adopting the arc ion plating technology. The invention has the advantages that: the coating is used on the surfaces of a cutter, a die and a core part, so that the coating has high hardness, lower friction coefficient, good high-temperature resistance and corrosion resistance, and the service life of a workpiece can be effectively prolonged.
Description
Technical Field
The invention relates to the field of vacuum coating, in particular to an AlTiSiCON superhard coating prepared by utilizing a vacuum ion plating technology and a specific preparation method thereof.
Background
The physical vapor deposition technology comprises evaporation plating, sputtering plating, ion plating and the like, and compared with the evaporation plating and the sputtering plating, the ion plating technology has the advantages of high ionization rate, good film-substrate binding force and the like. The research, development and application of the traditional ion plating technology are started from golden TiN coatings, and the requirements on the cutter are higher and higher along with the diversification of the processing environment of the cutter. High-quality cutters are always coated, the traditional single TiN coating cannot meet the requirement, and how to prepare high-performance hard coatings is the research and development direction of numerous business industries and research institutes.
The traditional TiN coating is generated by combining Ti target arc discharge and nitrogen, and various hard coatings are prepared industrially by preparing binary or ternary composite target materials of TiAl, AlTi, TiCr, AlCr and TiCrAl. Essentially, elements such as Cr, Al and the like are added into the TiN coating to improve the high temperature resistance and the corrosion resistance, and the microhardness is greatly improved and can reach more than HV 3000. In recent years, the addition of Si element into the coating is the key point of research, for example, the Si element is added into a more mature bronze TiSiN coating applied industrially, so that the crystal grains in the coating are finer, and the coating has the characteristics of high hardness and high toughness. The scholars add elements such as Si, O and the like into the coating containing Ti, Cr and Al, so that the surface of the coating forms a passive film under a high-temperature environment, the hardness and the toughness are not obviously reduced, and the application range of the coating is greatly widened.
In addition to changing or adding the components of the coating, the coating process is also very important, the preparation of the multilayer structure is helpful for reducing internal stress, and in the case of arc ion plating, large particles are easy to generate in the target material switching process, so that the more the film layers, the better. In addition, many parameters in the coating process also need to be designed carefully, and the parameters to be controlled include: baking temperature and time, gas type and pressure, workpiece bias, target current, coating time, workpiece rotation speed, target back magnetic field, cooling water temperature and the like.
Disclosure of Invention
The invention aims to provide an AlTiSiCON superhard coating prepared by using a vacuum ion plating technology and a specific preparation method thereof.
The invention adopts the following technical scheme to solve the technical problems:
an AlTiSiCON superhard coating is of a multilayer structure and sequentially comprises a TiN priming layer, an AlTiN layer, an AlTiSiCN layer and an AlTiSiCON surface layer from inside to outside; and the AlTiN layer, the AlTiSiCN layer, the AlTiN layer and the AlTiSiCN layer between the TiN priming layer and the AlTiSiCN surface layer form an AlTiN and AlTiSiCN staggered layer.
In a preferred embodiment of the present invention, the TiN primer layer has a thickness of 0.1 to 0.2 μm; the thickness of a single-layer AlTiN layer in the AlTiN and AlTiSiCN staggered layer is 0.1-0.3 mu m; the thickness of a single-layer AlTiSiCN layer in the AlTiN and AlTiSiCN staggered layer is 0.1-0.4 mu m; the thickness of the AlTiSiCON surface layer is 0.5-2.5 mu m.
In a preferred embodiment of the present invention, the AlTiN layer includes, in atomic number percentage: 25 to 30 percent of Ti; 40 to 50 percent of Al; 30-40% of N;
in the AlTiSiCN layer, the atomic number percentage is as follows: 20 to 25 percent of Ti; 35 to 45 percent of Al; si: 5% -10%; c: 5% -10%; 25 to 35 percent of N;
in the AlTiSiCON surface layer, the atomic number percentage is as follows: 15 to 25 percent of Ti; 30 to 40 percent of Al; si: 5% -10%; c: 5% -10%; o: 5% -10%; 25 to 35 percent of N.
As one of the preferable modes of the invention, the AlTiSiCON superhard coating is prepared by adopting an arc ion plating technology, and the preparation method comprises the following steps:
(1) ion cleaning
Installing the workpiece in a vacuum tank after clamping, filling Ar into the vacuum tank after air extraction and baking, wherein the gas flow is 50-100sccm, the gas pressure is 0.3-0.5Pa, starting an electron gun device to perform arc discharge, keeping the discharge current at 100 plus materials 150A, loading a negative bias voltage of 500 plus materials 850V on the surface of the workpiece, and starting ion cleaning for 20-60 minutes;
(2) preparation of TiN underlayer
Closing the electron gun, closing Ar gas, and filling N into the tank2The gas flow is 400-;
(3) preparing a staggered layer of AlTiN and AlTiSiCN
Turning off the Ti target, N2Adjusting the gas flow to be 500-1000sccm, the gas pressure to be 2-4Pa, reducing the workpiece bias voltage to 200V, starting the AlTi target, and preparing the AlTiN layer, wherein the target current is 80-105A and the time is 5-15 minutes; on the premise of keeping other parameters unchanged, N is added2Adjusting the gas flow to be 250-500sccm, simultaneously filling hexamethyldisilane HMDS into the vacuum tank, adjusting the steam flow to be 250-500sccm, keeping the total gas pressure at 2-3.5Pa for 5-15 minutes, and preparing an AlTiSiCN layer; repeating the steps to prepare an AlTiN and AlTiSiCN layer so as to form a staggered layer of the AlTiN and the AlTiSiCN;
(4) preparation of AlTiSiCON skin layer
On the premise of keeping other parameters unchanged, N is added2The gas flow is adjusted to 200-2The flow rate is 50-100sccm, the total gas pressure is 3-3.5Pa, the bias voltage is reduced to 100-150V, and the time is 25-90 minutes, so that the AlTiSiCON surface layer is prepared.
A preparation method of an AlTiSiCON superhard coating selects an arc ion plating technology, and comprises the following specific preparation steps:
(1) ion cleaning
Installing the workpiece in a vacuum tank after clamping, filling Ar into the vacuum tank after air extraction and baking, wherein the gas flow is 50-100sccm, the gas pressure is 0.3-0.5Pa, starting an electron gun device to perform arc discharge, keeping the discharge current at 100 plus materials 150A, loading a negative bias voltage of 500 plus materials 850V on the surface of the workpiece, and starting ion cleaning for 20-60 minutes;
(2) preparation of TiN underlayer
Closing the electron gun, closing Ar gas, and filling N into the tank2The gas flow is 400-;
(3) preparing a staggered layer of AlTiN and AlTiSiCN
Turning off the Ti target, N2Adjusting the gas flow to be 500-1000sccm, the gas pressure to be 2-4Pa, reducing the workpiece bias voltage to 200V, starting the AlTi target, and preparing the AlTiN layer, wherein the target current is 80-105A and the time is 5-15 minutes; on the premise of keeping other parameters unchanged, N is added2Adjusting the gas flow to be 250-500sccm, simultaneously filling hexamethyldisilane HMDS into the vacuum tank, adjusting the steam flow to be 250-500sccm, keeping the total gas pressure at 2-3.5Pa for 5-15 minutes, and preparing an AlTiSiCN layer; repeating the steps to prepare an AlTiN and AlTiSiCN layer so as to form a staggered layer of the AlTiN and the AlTiSiCN;
(4) preparation of AlTiSiCON skin layer
On the premise of keeping other parameters unchanged, N is added2The gas flow is adjusted to 200-2The flow rate is 50-100sccm, the total gas pressure is 3-3.5Pa, the bias voltage is reduced to 100-150V, and the time isAnd preparing an AlTiSiCON surface layer after 25-90 minutes.
As one of the preferred modes of the present invention, the raw materials used for the coating layer include AlTi target having an aluminum atom percentage content of 67%, Ti target, Hexamethyldisilane (HMDS), high purity nitrogen gas, high purity oxygen gas; wherein, AlN and Al are formed with higher aluminum content2O3The hard particles can refine coating grains, and the hardness, toughness, high temperature resistance and corrosion resistance of the coating can be improved to different degrees; four elements of Si, C, O and N in the coating are filled into the vacuum tank in a gaseous state or a steam state, and compared with a solid target material, the element content adjusting range is large, and the coatings with various performances can be prepared; si element and N, C, O and other elements form binary or multi-element nanocrystalline particles inside the coating, and crystal grains are further refined; the element C can reduce the friction coefficient of the coating, so that the cutter has higher cutting efficiency and smooth chip removal; o, N element is mainly used to form oxide, nitride, oxynitride, etc. with other elements to improve the comprehensive performance of the coating.
In a preferred embodiment of the present invention, the back magnetic field of the Ti target and the AlTi target of the coating is an electromagnetic plus permanent magnetic structure, and the electromagnetic field is adjusted in each furnace according to the consumption of the target material in order to ensure the uniformity of the coating quality.
As one of the preferable modes of the invention, the AlTiSiCON super-hard coating prepared by the preparation method can be used on the outer surfaces of cutters, moulds and core parts with high requirements on coating quality; the preparation process of the coating adopts a multilayer structure, and the internal stress of the coating can be effectively released, so that the coating is not easy to crack.
Compared with the prior art, the invention has the advantages that:
(1) the invention adopts the electric arc ion plating technology to prepare the AlTiSiCON superhard coating, and has the advantages of high ionization rate and good film-substrate binding force;
(2) the AlTiSiCON coating is composed of a TiN priming layer, an AlTiN layer, an AlTiSiCN layer and an AlTiSiCON surface layer multi-layer structure, the internal stress of the coating is effectively released, and the internal stress is lower;
(3) the traditional technology for preparing the multilayer film usually realizes the change of components by switching different target materials, however, large particles often and violently burst at the moment when the target materials are opened, which is unfavorable for the film layer, and the invention realizes the change of the components of the coating layers of different layers by changing the variety and the proportion of an air source under the condition of not changing the state of the target materials, thereby changing the growth mode of the film layer;
(4) the raw materials used by the invention comprise an AlTi target with the aluminum atom percentage content of 67%, a Ti target, Hexamethyldisilane (HMDS), high-purity nitrogen and high-purity oxygen; wherein, AlN and Al are formed with higher aluminum content2O3The hard particles can refine coating grains, and the hardness, toughness, high temperature resistance and corrosion resistance of the coating can be improved to different degrees; four elements of Si, C, O and N in the coating are filled into the vacuum tank in a gaseous state or a steam state, and compared with a solid target material, the element content adjusting range is large, and the coatings with various performances can be prepared; si element and N, C, O and other elements form binary or multi-element nanocrystalline particles inside the coating, and crystal grains are further refined; the element C can reduce the friction coefficient of the coating, so that the cutter has higher cutting efficiency and smooth chip removal; o, N element is mainly used to form oxide, nitride, oxynitride, etc. with other elements, thus improving the comprehensive performance of the coating;
(5) the back magnetic fields of the Ti target and the AlTi target used by the invention are electromagnetic and permanent magnetic structures, and in order to ensure the uniformity of the coating quality, the electromagnetic field is adjusted in each furnace according to the consumption of the target material.
Drawings
FIG. 1 is a schematic representation of the layered structure of the AlTiSiCON superhard coating of examples 1-3;
FIG. 2 is a view showing the structure of the back magnetic field of the AlTi target in example 7;
FIG. 3 is a view showing the structure of the magnetic field on the back of the Ti target in example 7;
FIG. 4 is an XRD phase diagram of the AlTiSiCON coating in example 7;
FIG. 5 is an SEM topography after high temperature treatment of the AlTiSiCN coating in example 7;
FIG. 6 is an SEM topography after high temperature treatment of the AlTiSiCON coating in example 7.
Detailed Description
The following examples are given for the detailed implementation and specific operation of the present invention, but the scope of the present invention is not limited to the following examples.
Example 1
The AlTiSiCON super-hard coating of the embodiment is 3-4 mu m thick and is suitable for a drill bit and the like.
The coating is of a multilayer structure and comprises a TiN priming layer, an AlTiN layer, an AlTiSiCN layer and an AlTiSiCN surface layer from inside to outside in sequence as shown in figure 1. The AlTiN layer, the AlTiSiCN layer, the AlTiN layer and the AlTiSiCN layer between the TiN priming layer and the AlTiSiCN surface layer integrally form an AlTiN and AlTiSiCN staggered layer.
Wherein, the thickness of the TiN priming coat is 0.1-0.2 μm; the thickness of a single-layer AlTiN layer in the staggered layer of the AlTiN and AlTiSiCN is 0.2-0.3 mu m; the thickness of a single-layer AlTiSiCN layer in the staggered layer of the AlTiN and AlTiSiCN is 0.2-0.4 mu m; the thickness of the AlTiSiCON surface layer is 1.0-2.5 μm.
Example 2
The AlTiSiCON super-hard coating of the embodiment has the thickness of 1.5-3 mu m, and is suitable for milling cutters, hobbing cutters, stamping dies and the like.
The coating is of a multilayer structure and comprises a TiN priming layer, an AlTiN layer, an AlTiSiCN layer and an AlTiSiCN surface layer from inside to outside in sequence as shown in figure 1. The AlTiN layer, the AlTiSiCN layer, the AlTiN layer and the AlTiSiCN layer between the TiN priming layer and the AlTiSiCN surface layer integrally form an AlTiN and AlTiSiCN staggered layer.
Wherein, the thickness of the TiN priming coat is 0.1-0.2 μm; the thickness of a single-layer AlTiN layer in the staggered layer of the AlTiN and AlTiSiCN is 0.15-0.2 mu m; the thickness of a single-layer AlTiSiCN layer in the staggered layer of the AlTiN and AlTiSiCN is 0.15-0.3 mu m; the thickness of the AlTiSiCON surface layer is 0.8-2.0 μm.
Example 3
The AlTiSiCON superhard coating is less than 1.5 mu m thick and is suitable for taps and the like with high precision requirement.
The coating is of a multilayer structure and comprises a TiN priming layer, an AlTiN layer, an AlTiSiCN layer and an AlTiSiCN surface layer from inside to outside in sequence as shown in figure 1. The AlTiN layer, the AlTiSiCN layer, the AlTiN layer and the AlTiSiCN layer between the TiN priming layer and the AlTiSiCN surface layer form an AlTiN and AlTiSiCN staggered layer.
Wherein, the thickness of the TiN priming coat is 0.1-0.2 μm; the thickness of a single-layer AlTiN layer in the staggered layer of the AlTiN and AlTiSiCN is 0.1-0.15 mu m; the thickness of a single-layer AlTiSiCN layer in the staggered layer of the AlTiN and AlTiSiCN is 0.1-0.2 mu m; the thickness of the AlTiSiCON surface layer is 0.5-1.0 μm.
Example 4
In the preparation method of the AlTiSiCON superhard coating in the embodiment 1, an arc ion plating technology is selected, and the specific preparation steps are as follows:
(1) ion cleaning
A workpiece is installed in a vacuum tank after being clamped, Ar is filled into the vacuum tank after air suction and baking, the gas flow is 100sccm, the gas pressure is 0.5Pa, an electron gun device is started to carry out arc discharge, the discharge current is kept at 150A, meanwhile, negative bias voltage 600V is loaded on the surface of the workpiece, and ion cleaning is started for 60 minutes;
(2) preparation of TiN underlayer
Closing the electron gun, closing Ar gas, and filling N into the tank2The gas flow is 400-600sccm, the gas pressure is 1.5-2.4Pa, the workpiece bias voltage is reduced to 300V, the Ti target is started, the target current is 80-90A, and the time is 5-10 minutes;
(3) preparing a staggered layer of AlTiN and AlTiSiCN
Turning off the Ti target, N2Adjusting the gas flow to be 700-800sccm, the gas pressure to be 2.8-3.2Pa, reducing the workpiece bias voltage to 200V, starting the AlTi target, and preparing the AlTiN layer, wherein the target current is 80-105A, and the time is 10-15 minutes; on the premise of keeping other parameters unchanged, N is added2Adjusting the gas flow to be 250-300sccm, simultaneously filling hexamethyldisilane HMDS into the vacuum tank, controlling the steam flow to be 250-300sccm, controlling the total gas pressure to be 2-3Pa, and controlling the time to be 10-15 minutes, thereby preparing an AlTiSiCN layer; repeating the steps to prepare an AlTiN and AlTiSiCN layer so as to form a staggered layer of the AlTiN and the AlTiSiCN;
(4) preparation of AlTiSiCON skin layer
On the premise of keeping other parameters unchanged, N is added2The gas flow rate is adjusted to 200-2The flow rate is 50-100sccm, the total gas pressure is 3-3.5Pa, the bias voltage is reduced to 100-150V, and the time is 30-90 minutes, so that the AlTiSiCON surface layer is prepared.
Further, the coating uses raw materials including an AlTi target having an aluminum atom percentage content of 67%, a Ti target, Hexamethyldisilane (HMDS), high purity nitrogen gas, high purity oxygen gas; wherein, AlN and Al are formed with higher aluminum content2O3The hard particles can refine coating grains, and the hardness, toughness, high temperature resistance and corrosion resistance of the coating can be improved to different degrees; four elements of Si, C, O and N in the coating are filled into the vacuum tank in a gaseous state or a steam state, and compared with a solid target material, the element content adjusting range is large, and the coatings with various performances can be prepared; si element and N, C, O and other elements form binary or multi-element nanocrystalline particles inside the coating, and crystal grains are further refined; the element C can reduce the friction coefficient of the coating, so that the cutter has higher cutting efficiency and smooth chip removal; o, N element is mainly used to form oxide, nitride, oxynitride, etc. with other elements to improve the comprehensive performance of the coating.
Further, the back magnetic fields of the Ti target and the AlTi target of the coating are of an electromagnetic and permanent magnet structure, and in order to ensure the uniformity of the coating quality, the electromagnetic field is adjusted in each furnace according to the consumption of the target material.
Example 5
In the preparation method of the AlTiSiCON superhard coating in the embodiment 2, an arc ion plating technology is selected, and the specific preparation steps are as follows:
(1) ion cleaning
Installing a workpiece in a vacuum tank after clamping, filling Ar into the vacuum tank after air suction and baking, wherein the gas flow is 75sccm, the gas pressure is 0.4Pa, starting an electron gun device to perform arc discharge, keeping the discharge current at 120A, loading a negative bias voltage 650V on the surface of the workpiece, and starting ion cleaning for 50 minutes;
(2) preparation of TiN underlayer
Closing the electron gun, closing Ar gas, and filling N into the tank2The gas flow is 400-;
(3) preparing a staggered layer of AlTiN and AlTiSiCN
Turning off the Ti target, N2Adjusting the gas flow to be 500-1000sccm, the gas pressure to be 2-4Pa, reducing the workpiece bias voltage to 200V, starting the AlTi target, and preparing the AlTiN layer, wherein the target current is 80-105A and the time is 8-10 minutes; on the premise of keeping other parameters unchanged, N is added2Adjusting the gas flow to be 250-plus 500sccm, simultaneously filling hexamethyldisilane HMDS into the vacuum tank, controlling the steam flow to be 250-plus 300sccm, controlling the total gas pressure to be 2-3Pa, and controlling the time to be 8-10 minutes to prepare an AlTiSiCN layer; repeating the steps to prepare an AlTiN and AlTiSiCN layer so as to form a staggered layer of the AlTiN and the AlTiSiCN;
(4) preparation of AlTiSiCON skin layer
On the premise of keeping other parameters unchanged, N is added2The gas flow rate is adjusted to 200-2The flow rate is 50-100sccm, the total gas pressure is 3-3.5Pa, the bias voltage is reduced to 100-150V, and the time is 30-70 minutes, so that the AlTiSiCON surface layer is prepared.
Further, the coating uses raw materials including an AlTi target having an aluminum atom percentage content of 67%, a Ti target, Hexamethyldisilane (HMDS), high purity nitrogen gas, high purity oxygen gas; wherein, AlN and Al are formed with higher aluminum content2O3The hard particles can refine coating grains, and the hardness, toughness, high temperature resistance and corrosion resistance of the coating can be improved to different degrees; four elements of Si, C, O and N in the coating are filled into the vacuum tank in a gaseous state or a steam state, and compared with a solid target material, the element content adjusting range is large, and the coatings with various performances can be prepared; si element and N, C, O and other elements form binary or multi-element nanocrystalline particles inside the coating, and crystal grains are further refined; the element C can reduce the friction coefficient of the coating, so that the cutter has higher cutting efficiency and smooth chip removal; o, N element ofThe coating mainly has the effect of forming oxides, nitrides, nitrogen oxides and the like with other elements, and the comprehensive performance of the coating is improved.
Further, the back magnetic fields of the Ti target and the AlTi target of the coating are of an electromagnetic and permanent magnet structure, and in order to ensure the uniformity of the coating quality, the electromagnetic field is adjusted in each furnace according to the consumption of the target material.
Example 6
In the preparation method of the AlTiSiCON superhard coating in the embodiment 3, an arc ion plating technology is selected, and the specific preparation steps are as follows:
(1) ion cleaning
Installing a workpiece in a vacuum tank after clamping, filling Ar into the vacuum tank after air suction and baking, wherein the gas flow is 100sccm, the gas pressure is 0.5Pa, starting an electron gun device to perform arc discharge, keeping the discharge current at 100A, loading a negative bias voltage of 500V on the surface of the workpiece, and starting ion cleaning for 40 minutes;
(2) preparation of TiN underlayer
Closing the electron gun, closing Ar gas, and filling N into the tank2The gas flow is 700-;
(3) preparing a staggered layer of AlTiN and AlTiSiCN
Turning off the Ti target, N2Adjusting the gas flow to be 800-sccm, the gas pressure to be 3.5-4Pa, reducing the workpiece bias voltage to 200V, starting the AlTi target, the target current to be 80-85A, and the time to be 5-8 minutes to prepare an AlTiN layer; on the premise of keeping other parameters unchanged, N is added2Adjusting the gas flow to be 400-500sccm, simultaneously filling hexamethyldisilane HMDS into the vacuum tank, wherein the steam flow is 400-500sccm, the total gas pressure is 3.5Pa, and the time is 5-8 minutes, and preparing an AlTiSiCN layer; repeating the steps to prepare an AlTiN and AlTiSiCN layer so as to form a staggered layer of the AlTiN and the AlTiSiCN;
(4) preparation of AlTiSiCON skin layer
On the premise of keeping other parameters unchanged, N is added2The gas flow rate is adjusted to 300-2The flow rate is 50-100sccm, the total gas pressure is 3-3.5Pa, the bias voltage is reduced to 100-150V, and the time is 20-40 minutes, so that the AlTiSiCON surface layer is prepared.
Further, the coating uses raw materials including an AlTi target having an aluminum atom percentage content of 67%, a Ti target, Hexamethyldisilane (HMDS), high purity nitrogen gas, high purity oxygen gas; wherein, AlN and Al are formed with higher aluminum content2O3The hard particles can refine coating grains, and the hardness, toughness, high temperature resistance and corrosion resistance of the coating can be improved to different degrees; four elements of Si, C, O and N in the coating are filled into the vacuum tank in a gaseous state or a steam state, and compared with a solid target material, the element content adjusting range is large, and the coatings with various performances can be prepared; si element and N, C, O and other elements form binary or multi-element nanocrystalline particles inside the coating, and crystal grains are further refined; the element C can reduce the friction coefficient of the coating, so that the cutter has higher cutting efficiency and smooth chip removal; o, N element is mainly used to form oxide, nitride, oxynitride, etc. with other elements to improve the comprehensive performance of the coating.
Further, the back magnetic fields of the Ti target and the AlTi target of the coating are of an electromagnetic and permanent magnet structure, and in order to ensure the uniformity of the coating quality, the electromagnetic field is adjusted in each furnace according to the consumption of the target material.
Example 7
This example illustrates the detailed parameter design and coating performance analysis of the AlTiSiCON superhard coating in the above examples.
The AlTiSiCON coating comprises the following components in parts by weight:
the layered structure of the AlTiSiCON coating of the invention is shown in figure 1, and the composition of each layered structure is shown in table 1. Most of the coatings are damaged layer by layer from the surface, in order to improve the durability of the coatings and reduce the internal stress, the invention adopts a multilayer structure, wherein an AlTiN layer, an AlTiSiCN layer, an AlTiN layer and an AlTiSiCN layer between a TiN priming layer and an AlTiSiCN surface layer belong to the interleaving of the AlTiN layer and the AlTiSiCN layer, so the coating is called an interleaving layer of the AlTiN and the AlTiSiCN; the thickness of the TiN priming layer is 0.1-0.2 μm, the thickness of a single-layer AlTiN layer in the AlTiN and AlTiSiCN staggered layer is 0.1-0.3 μm, the thickness of a single-layer AlTiSiCN layer in the AlTiN and AlTiSiCN staggered layer is 0.1-0.4 μm, and the thickness of the AlTiSiCON surface layer is 0.5-2.5 μm.
TABLE 1 AlTiSiCON nanocomposite coating layered composition (at.%)
| Coating (layers) | Ti | Al | Si | C | N | O |
| TiN base coat | 45-55 | 0 | 0 | 0 | 35-45 | 0 |
| AlTiN layer | 25-30 | 40-50 | 0 | 0 | 30-40 | 0 |
| AlTiSiCN layer | 20-25 | 35-45 | 5-10 | 5-10 | 25-35 | 0 |
| AlTiN layer | 25-30 | 40-50 | 0 | 0 | 30-40 | 0 |
| AlTiSiCN layer | 20-25 | 35-45 | 5-10 | 5-10 | 25-35 | 0 |
| AlTiSiCON skin layer | 15-25 | 30-40 | 5-10 | 5-10 | 25-35 | 5-10 |
Setting the current of the electromagnetic coil of the target material and the size of the central magnetic field of the target surface:
the back magnetic field structure of the target of the invention is shown in figures 2-3 (figure 2 is the back magnetic field structure of the AlTi target, figure 3 is the back magnetic field structure of the Ti target), and the current settings of the electromagnetic coils of the target of different heats and the size of the central magnetic field of the target surface are shown in table 2. As is well known, the target material can be continuously consumed in the film coating process by the ion plating technology, no matter what type of magnetic field is adopted at the back of the target material, the magnetic field of the target surface can be stronger and stronger along with the thinning of the target material, the utilization rate of the target material can be reduced by local ablation, and the product quality of each furnace is different. The back of the Ti target and the back of the AlTi target are provided with the electromagnetic and permanent magnet structures, the electromagnetic coil is arranged in the center of the target, and the permanent magnets are uniformly arranged on the edge of the target to form a circular structure. The magnetic field of the permanent magnet cannot be changed, the magnetic field is changed by adjusting the current of the electromagnetic coil, and the electromagnetic field and the magnetic field of the permanent magnet are coupled and then act on the surface of the target. The polarity of the magnetic field generated by the electromagnetic coil in the Ti target is the same as that of the magnetic field and the magnetic field of the permanent magnet at the edge, and the current of the coil needs to be increased to keep balance as the target material is consumed and becomes thinner; the polarity of the electromagnetic coil generated in AlTi is opposite to that of the magnetic field generated by the magnetic field and the magnetic field of the permanent magnet at the edge, and the current of the coil needs to be reduced to keep balance as the target material is consumed and becomes thinner. Along with the change of the magnetic field, the ablation position of the target surface gradually expands outwards, so that the utilization rate of the target material is improved.
TABLE 2 electromagnetic coil current settings and central magnetic field of target surface for different heats of target material
Thirdly, comparing the performance parameters of each coating:
in this example, 5 composite coatings of AlTiN, AlTiCN, AlTiSiCN, TiAlSiCON coating (low aluminum content), AlTiSiCON coating (high aluminum content, i.e., the AlTiSiCON superhard coating described in examples 1 to 6) were prepared on the surface of H13 steel by a controlled variable method, that is, on the premise that the coating process parameters were the same, the effect of a certain component in the coating was analyzed by changing the component, and the specific results are shown in table 3. Wherein: the hardness of the coating is measured by adopting an HV-1000 type micro Vickers hardness tester, and the loading load is 50 g; testing the dry friction coefficient and the grinding mark size of the coating by using an ISC-200 type needle disc type friction wear testing machine and an optical microscope, wherein the grinding material is an alumina ball; the composition is obtained by EDS energy spectrum test; and scanning the surface of the sample by using a KRISTALLOFLEX 805 XRD diffractometer produced by Siemens company, and analyzing and comparing the data by using a D500 goniometer to obtain the phase composition and the grain size of the coating.
Table 3 is a comparison of the performance parameters of each coating, and a smaller wear scar size means that the coating is more wear resistant. In general, the introduction of Si element can make the crystal particles of the coating finer and the hardness higher. According to the fine grain strengthening theory, the coating has better toughness, so the coating is more wear-resistant. The element C can reduce the friction coefficient of the coating, so that the friction resistance of the coating in the working process is smaller, and the machining efficiency is high. The high aluminum content in the coating increases the hardness of the coating, and the grain size is smaller, which reduces wear.
TABLE 3 comparison of the Property parameters of the coatings
Fourthly, XRD phase diagram analysis of the AlTiSiCON coating of the invention:
FIG. 4 is an XRD phase diagram of the AlTiSiCON coating of the present invention. It can be seen that: the coating does not have the crystal structure of nitrides and oxides of Al, and the nitrides, oxides and carbides of Al are likely to exist in the coating in an amorphous form in the coating process, and the superhard phase of the amorphous aluminide mixed crystal state can greatly influence the high-temperature performance of the coating.
And fifthly, the SEM appearance comparative analysis of the AlTiSiCN coating of the invention after high temperature treatment with the AlTiSiCN coating is as follows:
FIG. 5 is a SEM topography after high temperature treatment of the AlTiSiCN coating of the invention; FIG. 6 is an SEM topography after high temperature treatment of the AlTiSiCON coating. It can be seen that: flocculent oxide skin appears on the surface of the AlTiSiCN coating after high-temperature treatment, which shows that the coating structure is damaged at high temperature, and the use function of the coating is greatly influenced; after the AlTiSiCON coating is treated at high temperature, no obvious oxide skin is generated on the surface, the structure is still compact, and the fact that the high-temperature resistance of the coating can be obviously improved by adding the oxygen element into the coating is shown.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents and improvements made within the spirit and principle of the present invention are intended to be included within the scope of the present invention.
Claims (6)
1. The AlTiSiCON superhard coating is characterized in that the coating is of a multilayer structure and sequentially comprises a TiN priming layer, an AlTiN layer, an AlTiSiCN layer and an AlTiSiCON surface layer from inside to outside; the AlTiN layer, the AlTiSiCN layer, the AlTiN layer and the AlTiSiCN layer between the TiN priming layer and the AlTiSiCN surface layer form an AlTiN and AlTiSiCN staggered layer;
and in the AlTiN layer, the atomic number percentage is as follows: 25 to 30 percent of Ti; 40 to 50 percent of Al; 30-40% of N;
in the AlTiSiCN layer, the atomic number percentage is as follows: 20 to 25 percent of Ti; 35 to 45 percent of Al; si: 5% -10%; c: 5% -10%; 25 to 35 percent of N;
in the AlTiSiCON surface layer, the atomic number percentage is as follows: 15 to 25 percent of Ti; 30 to 40 percent of Al; si: 5% -10%; c: 5% -10%; o: 5% -10%; 25 to 35 percent of N.
2. The AlTiSiCON superhard coating of claim 1, wherein the TiN primer layer has a thickness of 0.1-0.2 μ ι η; the thickness of a single-layer AlTiN layer in the AlTiN and AlTiSiCN staggered layer is 0.1-0.3 mu m; the thickness of a single-layer AlTiSiCN layer in the AlTiN and AlTiSiCN staggered layer is 0.1-0.4 mu m; the thickness of the AlTiSiCON surface layer is 0.5-2.5 mu m.
3. The AlTiSiCON superhard coating of any one of claims 1 to 2, wherein the AlTiSiCON superhard coating is prepared by arc ion plating technology by the following method:
(1) ion cleaning
Installing the workpiece in a vacuum tank after clamping, filling Ar into the vacuum tank after air extraction and baking, wherein the gas flow is 50-100sccm, the gas pressure is 0.3-0.5Pa, starting an electron gun device to perform arc discharge, keeping the discharge current at 100 plus materials 150A, loading a negative bias voltage of 500 plus materials 850V on the surface of the workpiece, and starting ion cleaning for 20-60 minutes;
(2) preparation of TiN underlayer
Closing the electron gun, closing Ar gas, and filling N into the tank2The gas flow is 400-;
(3) preparing a staggered layer of AlTiN and AlTiSiCN
Turning off the Ti target, N2Adjusting the gas flow to be 500-1000sccm, the gas pressure to be 2-4Pa, reducing the workpiece bias voltage to 200V, starting the AlTi target, and preparing the AlTiN layer, wherein the target current is 80-105A and the time is 5-15 minutes; on the premise of keeping other parameters unchanged, N is added2Adjusting the gas flow to be 250-500sccm, simultaneously filling hexamethyldisilane HMDS into the vacuum tank, adjusting the steam flow to be 250-500sccm, keeping the total gas pressure at 2-3.5Pa for 5-15 minutes, and preparing an AlTiSiCN layer; repeating the steps to prepare an AlTiN and AlTiSiCN layer so as to form a staggered layer of the AlTiN and the AlTiSiCN;
(4) preparation of AlTiSiCON skin layer
On the premise of keeping other parameters unchanged, N is added2The gas flow is adjusted to 200-2The flow rate is 50-100sccm, the total gas pressure is 3-3.5Pa, the bias voltage is reduced to 100-150V, and the time is 25-90 minutes, so that the AlTiSiCON surface layer is prepared.
4. A method for preparing an AlTiSiCON superhard coating according to any one of claims 1 to 3, wherein an arc ion plating technique is selected, and the specific preparation steps are as follows:
(1) ion cleaning
Installing the workpiece in a vacuum tank after clamping, filling Ar into the vacuum tank after air extraction and baking, wherein the gas flow is 50-100sccm, the gas pressure is 0.3-0.5Pa, starting an electron gun device to perform arc discharge, keeping the discharge current at 100 plus materials 150A, loading a negative bias voltage of 500 plus materials 850V on the surface of the workpiece, and starting ion cleaning for 20-60 minutes;
(2) preparation of TiN underlayer
Closing the electron gun, closing Ar gas, and filling N into the tank2The gas flow is 400-;
(3) preparing a staggered layer of AlTiN and AlTiSiCN
Turning off the Ti target, N2Adjusting the gas flow to be 500-1000sccm, the gas pressure to be 2-4Pa, reducing the workpiece bias voltage to 200V, starting the AlTi target, and preparing the AlTiN layer, wherein the target current is 80-105A and the time is 5-15 minutes; on the premise of keeping other parameters unchanged, N is added2Adjusting the gas flow to be 250-500sccm, simultaneously filling hexamethyldisilane HMDS into the vacuum tank, adjusting the steam flow to be 250-500sccm, keeping the total gas pressure at 2-3.5Pa for 5-15 minutes, and preparing an AlTiSiCN layer; repeating the steps to prepare an AlTiN and AlTiSiCN layer so as to form a staggered layer of the AlTiN and the AlTiSiCN;
(4) preparation of AlTiSiCON skin layer
On the premise of keeping other parameters unchanged, N is added2The gas flow is adjusted to 200-2The flow rate is 50-100sccm, the total gas pressure is 3-3.5Pa, the bias voltage is reduced to 100-150V, and the time is 25-90 minutes, so that the AlTiSiCON surface layer is prepared.
5. The method for preparing the AlTiSiCON superhard coating according to claim 4, wherein the Ti target and the AlTi target have electromagnetic and permanent magnet structures on the back.
6. The method for preparing an AlTiSiCON superhard coating according to claim 4, wherein the AlTiSiCON coating prepared by the preparation method is applied to the outer surfaces of cutters, molds and core parts.
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