CN110484870B - Multicomponent nitride hard coating and preparation method and application thereof - Google Patents
Multicomponent nitride hard coating and preparation method and application thereof Download PDFInfo
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- CN110484870B CN110484870B CN201910754387.2A CN201910754387A CN110484870B CN 110484870 B CN110484870 B CN 110484870B CN 201910754387 A CN201910754387 A CN 201910754387A CN 110484870 B CN110484870 B CN 110484870B
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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
- C23C14/0021—Reactive sputtering or evaporation
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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
- C23C14/06—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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- 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
Abstract
The invention belongs to the field of surface protection coating materials, and discloses a multi-component nitride hard coating, and a preparation method and application thereof. The hard coating comprises a (TiAlCrTaW) N layer, wherein the (TiAlCrTaW) N layer is in a columnar crystal growth structure, and the chemical formula of the (TiAlCrTaW) N layer is (Ti)aAlbCrcTadWe) N, wherein a + b + c + d + e is 1; a is more than or equal to 0.2 and less than or equal to 0.5; b is more than or equal to 0.2 and less than or equal to 0.5; c is more than or equal to 0 and less than or equal to 0.2; d is more than or equal to 0 and less than or equal to 0.2; e is more than or equal to 0 and less than or equal to 0.2. The hard coating has excellent high-temperature structure, mechanical stability, oxidation resistance and abrasion resistance; the hardness value in a deposition state is 30-40 GPa, and the elastic modulus is 400-500 GPa; the hardness value at 900 ℃ is 35-45 GPa, and the elastic modulus is 450-550 GPa.
Description
Technical Field
The invention belongs to the technical field of material science and engineering, and particularly relates to a multi-component nitride hard coating as well as a preparation method and application thereof.
Background
With the rapid development of modern cutting techniques, particularly high-speed cutting and dry cutting, higher requirements are placed on the performance and service environment of cutting tools. The coated cutter combines the advantages of high hardness, high wear resistance and low friction coefficient of a surface coating and high toughness and high strength of a substrate, greatly improves the cutting performance of the cutter, improves the processing efficiency, and reduces diffusion and chemical reaction between the cutter and a workpiece by using the coating material as a chemical barrier and a thermal barrier, thereby reducing the abrasion of the cutter, prolonging the service life of the cutter and becoming the center of gravity of the modern cutting technology.
Metastable-phase MeAlN coatings formed by replacing part of Me in transition metal nitride MeN (Me ═ Ti, Cr and the like) by Al have high hardness, high melting point and good oxidation resistance and are widely used as cutter coating materials, wherein TiAlN coatings have good red hardness, and CrAlN has excellent oxidation resistance. With the continuous updating of industrial materials, the cutting processing and forming of some difficult-to-process materials are particularly involved, and the local service temperature is higher than 900 ℃. The severe high temperature service environment can lead to phase decomposition of the MeAlN coating, and simultaneously, the oxidation resistance is sharply reduced, and finally, the premature failure of the coated cutter is caused. This places higher demands on the high temperature resistance of the tool coating, in particular on the thermal stability and oxidation resistance and on the high temperature wear resistance.
The improvement of tool coating properties (e.g., TiAlN coatings) by the addition of alloying elements (V, Cr, Y, W, Ta, etc.) is becoming an important direction of tool coating research. For example, the oxidation resistance of the TiAlN coating can be improved by introducing Cr; the introduction of Ta has a remarkable influence on the thermal stability; the addition of W can significantly improve the wear resistance. However, the addition of a single alloying element has certain limitations on the improvement of the coating properties, such as poor thermal stability due to excessive Cr addition. In order to achieve comprehensive improvement of the coating performance of the cutter, a method for improving the coating performance by multi-component alloying is attracting attention.
Disclosure of Invention
In order to solve the above-mentioned disadvantages and drawbacks of the prior art, a primary object of the present invention is to provide a multi-component nitride hard coating. The coating has excellent high-temperature thermal stability, high-temperature oxidation resistance and wear resistance.
The invention also aims to provide a preparation method of the multicomponent nitride hard coating. The method is based on a cathode arc evaporation deposition technology, and the components of the coating are adjusted by adjusting the component proportion of the alloy target.
The invention also aims to provide application of the multicomponent nitride hard coating.
The purpose of the invention is realized by the following technical scheme:
a multi-component nitride hard coating comprises a (TiAlCrTaW) N layer, wherein the (TiAlCrTaW) N layer has a columnar crystal growth structure, and the chemical formula of the (TiAlCrTaW) N layer is (Ti)aAlbCrcTadWe) N, wherein a + b + c + d + e is 1; a is more than or equal to 0.2 and less than or equal to 0.5; b is more than or equal to 0.2 and less than or equal to 0.5; c is more than or equal to 0 and less than or equal to 0.2; d is more than or equal to 0 and less than or equal to 0.2; e is more than or equal to 0 and less than or equal to 0.2.
Preferably, the hardness value of the hard coating in a deposition state is 30-40 GPa, and the elastic modulus is 400-500 GPa.
Preferably, the hardness value of the hard coating at 900 ℃ is 35-45 GPa, and the elastic modulus is 450-550 GPa.
The multicomponent nitride hard coating comprises the following specific steps:
s1, putting the cleaned and dried substrate material into a PVD vacuum coating chamber, and vacuumizing to 1-6 multiplied by 10-3Pa；
S2, heating the cavity to 300-400 ℃, keeping the temperature constant, introducing Ar gas to adjust the air pressure of the cavity, and performing high-energy beam ion etching cleaning on the substrate;
s3, closing the Ar gas valve and introducing N2Adjusting the air pressure of the chamber, igniting the corresponding target by adopting a cathodic arc evaporation deposition method, setting the target current, setting the bias voltage to be-80 to-150V under the nitrogen atmosphere, and depositing (Ti)aAlbCrcTadWe) And N coating to obtain the multicomponent nitride hard coating.
Preferably, the base material in step S1 is cemented carbide or high-speed steel.
More preferably, the hard alloy is WC-Co-TiC, WC-Co, WC-TiC-TaC (NbC) -Co alloy.
Preferably, the chamber pressure in step S2 is 0.5-1 Pa.
Preferably, in step S3, the chamber pressure is 2-4 Pa, and the target current is 65-95A.
Preferably, the deposition time in the step S3 is 60-120 min.
The multicomponent nitride hard coating is applied to the fields of turning, milling and drilling.
Based on the cathodic arc evaporation deposition technology, the invention realizes component regulation and control by a multi-alloying way, and obtains the Ti with excellent high-temperature thermal stability, high-temperature oxidation resistance and wear resistanceaAlbCrcTadWe) And (3) N hard coating. The regulation and control of coating components are realized through the component design of the target material, and the introduction of Cr alloy elements on the basis of the TiAlN coating can promote the surface densification (Al, Cr) of the coating at high temperature2O3The formation of oxide, which effectively prevents the further oxidation of the coating; ta alloy element is introduced, so that the polymerization energy of a coating system can be obviously improved, the coating can keep good structural stability at high temperature, the defect of poor thermal stability caused by single Cr alloying is overcome, and meanwhile, Ta element can form complementary action with Cr element in the aspect of oxidation resistance, so that (Ti) is formedaAlbCrcTadWe) The N keeps excellent oxidation resistance in a larger temperature window, and makes up for the oxidation resistance deterioration of single Cr alloying in a high temperature section (particularly the temperature is more than or equal to 900 ℃); the W element can generate a magneli phase on the surface in the friction process, and the friction coefficient of the coating is remarkably reduced, so that (Ti)aAlbCrcTadWe) N exhibits excellent wear resistance. Through a pair (Ti)aAlbCrcTadWe) The composition of the N coating is designed such that (Ti)aAlbCrcTadWe) The N hard coating layer shows excellent combination properties such as high temperature stability, high temperature oxidation resistance and abrasion resistance at the temperature higher than 900 DEG CCan further enrich the selection system of the cutter coating and meet the requirements of modern cutting processing.
Compared with the prior art, the invention has the following beneficial effects:
1. of the invention (Ti)aAlbCrcTadWe) The N hard coating shows that a polycrystalline structure grows in a columnar crystal form, and has excellent high-temperature thermal stability, high-temperature oxidation resistance and wear resistance under the condition that the service temperature is higher than 900 ℃.
2. Compared with a MeAlN (Me ═ Ti and Cr) coating, the multi-element nitride hard coating can obviously delay the phase transition temperature of the coating at high temperature, improve the high-temperature thermal stability of the coating and enable the coating to show obvious aging strengthening effect; meanwhile, a good oxygen diffusion barrier layer is formed on the surface of the coating, so that the oxidation process at high temperature is slowed down, and the coating has excellent oxidation resistance in a wider temperature window; the generation of the lubricating phase during the friction process obviously improves the wear resistance of the coating.
3. The preparation method disclosed by the invention is simple, strong in operability and good in controllability, is suitable for protecting the surfaces of products such as mechanical parts, knives/molds and the like, and has good economic benefits.
Drawings
FIG. 1 is an XRD pattern of the TiAlCrN, TiAlCrTaN and TiAlCrTaWN hard coatings of examples 1-3.
FIG. 2 shows the cross-sectional secondary electron morphology of the hard coatings of TiAlCrN, TiAlCrTaN and TiAlCrTaWN in examples 1-3.
FIG. 3 is the XRD patterns of the TiAlCrN, TiAlCrTaN and TiAlCrTaWN hard coatings of examples 1-3 after vacuum annealing at different temperatures.
FIG. 4 shows (a) nanoindentation hardness and (b) elastic modulus of the hard coatings of examples 1-3 after vacuum annealing at different temperatures.
FIG. 5 is a scanning electron microscope image of fracture cross section of the hard coatings of TiAlCrN, TiAlCrTaN and TiAlCrTaWN in examples 1-3 after constant temperature oxidation for 5h at different temperatures.
Detailed Description
The following examples are presented to further illustrate the present invention and should not be construed as limiting the invention. Unless otherwise specified, the technical means used in the examples are conventional means well known to those skilled in the art. Reagents, methods and apparatus used in the present invention are conventional in the art unless otherwise indicated.
The invention is based on a cathode arc evaporation deposition technology, and different multi-component alloying hard coatings are prepared in a nitrogen environment by using PVD vacuum coating equipment (GDUT-HAS 500). Wherein seven alloy targets with different component ratios are used for preparing (TiAlCrTaW) N coatings with corresponding components, and the target components are respectively Ti50Al50、Ti40Al50Cr10、Ti30Al50Cr10Ta10、Ti30Al50Cr10W10、Ti20Al20Cr20Ta20W20、Ti30Al30Cr20Ta10W10、Ti25Al30Cr15Ta15W15。
Example 1
Polishing a hard alloy matrix (WC-8 wt.% Co-4 wt.% TiC), ultrasonically cleaning the hard alloy matrix for 60min by acetone and absolute ethyl alcohol, blow-drying the hard alloy matrix by using common nitrogen, and then putting the hard alloy matrix on a tray of a vacuum chamber. Turning on a heater, heating to 350 deg.C, turning on a vacuum system during heating, and vacuumizing the chamber to a vacuum degree of 5 × 10-3Pa or less. Introducing Ar gas, adjusting the pressure of the cavity to 0.55Pa, performing high-energy beam ion etching cleaning on the substrate, closing an Ar gas valve, and introducing N2The gas flow rate was 300sccm and the chamber pressure was controlled to 3 Pa. Adjusting the bias voltage of the workpiece rotating stand to-100V, igniting Ti40Al50Cr10Setting the target current to be 80A, depositing for 60min, and preparing Ti on the surface of the hard alloy substrate0.42Al0.47Cr0.11N hard coating (labeled TiAlCrN).
Example 2
The difference from the embodiment 1 is that: the alloy target is Ti30Al50Cr10Ta10Target, prepared with a coating of Ti0.34Al0.48Cr0.11Ta0.07N (labeled TiAlCrTaN).
Example 3
The difference from the embodiment 1 is that: the alloy target is Ti20Al20Cr20Ta20W20Target, prepared with a coating of Ti0.20Al0.20Cr0.20Ta0.20W0.20N (labeled TiAlCrTaWN).
Example 4
The difference from the embodiment 1 is that: the alloy target is Ti30Al50Cr10W10Target, prepared with a coating of Ti0.34Al0.47Cr0.11W0.08N。
Example 5
The difference from the embodiment 1 is that the alloy target material is Ti30Al30Cr20Ta10W10Target, prepared with a coating of Ti0.30Al0.30Cr0.20Ta0.10W0.10N。
Example 6
The difference from the embodiment 1 is that the alloy target material is Ti25Al30Cr15Ta15W15Target, prepared with a coating of Ti0.25Al0.30Cr0.15Ta0.15W0.15N。
Comparative example 1
The difference from the embodiment 1 is that: the alloy target is Ti50Al50Target, prepared with a coating of Ti0.50Al0.50N。
The chemical compositions of seven different target compositions and corresponding coatings in examples 1-6 and comparative example 1 are shown in table 1.
TABLE 1 target composition and corresponding coating chemistry
In the invention, a scanning electron microscope (FEI Nova NanoSEM 430) is used for observing and analyzing the cross-sectional morphology of the coating; performing a vacuum heat treatment experiment by using a high-temperature vacuum annealing furnace, selecting heat treatment temperatures of 700 ℃, 800 ℃, 900 ℃, 1000 ℃, 1100 ℃, a heating rate of 10K/min, keeping the temperature for 30min, adopting a furnace cooling mode, then representing a coating deposition state and an annealed phase structure by using an X-ray diffractometer (BRUKER D8), and representing the hardness and the elastic modulus of an annealed sample by using a nano indenter in a constant load mode; and (3) carrying out constant temperature oxidation experiments at 850 ℃ and 900 ℃ on the coating sample, wherein the constant temperature duration is 5h, and representing the oxidation section by utilizing a scanning electron microscope.
FIG. 1 shows Ti in examples 1 to 30.42Al0.47Cr0.11N(TiAlCrN)、Ti0.34Al0.48Cr0.11Ta0.07N (TiAlCrTaN) and Ti0.20Al0.20Cr0.20Ta0.20W0.20An XRD pattern of a deposited state of an N (TiAlCrTaWN) coating, all coatings show a typical face-centered cubic structure, and compared with the TiAlN coating in comparative example 1, the introduced alloying elements Cr, Ta and W exist in a solid solution form, so that the diffraction front is shifted to a high angle; FIG. 2 shows Ti in examples 1 to 30.42Al0.47Cr0.11N、Ti0.34Al0.48Cr0.11Ta0.07N and Ti0.20Al0.20Cr0.20Ta0.20W0.20The cross section of the N coating has secondary electron morphology, and the three coatings have obvious columnar crystal growth morphology.
FIG. 3 shows Ti in examples 1 to 30.42Al0.47Cr0.11N、Ti0.34Al0.48Cr0.11Ta0.07N and Ti0.20Al0.20Cr0.20Ta0.20W0.20XRD pattern of N coating after annealing at 700 deg.C, 800 deg.C, 900 deg.C, 1000 deg.C, 1100 deg.C. Ti relative to TiAlN coating in comparative example 10.42Al0.47Cr0.11N and Ti0.34Al0.48Cr0.11Ta0.07The N coating started to appear w-AlN at 900 ℃ and 1000 ℃ respectively, while Ti0.20Al0.20Cr0.20Ta0.20W0.20The N coating can significantly delay the generation temperature of w-AlN to 1100 ℃, wherein the generation of w-AlN can have adverse effect on the mechanical property of the coating. Further, Ti0.34Al0.48Cr0.11Ta0.07N and Ti0.20Al0.20Cr0.20Ta0.20W0.20The thermal decomposition process of the N coating is also inhibited to a certain extent, and the nano hardness and elastic modulus characterization curves corresponding to the graph in FIG. 4 show that the Ti reflects the mechanical property expression0.20Al0.20Cr0.20Ta0.20W0.20The hardness value of the N coating in a deposition state is 34.3GPa, the elastic modulus is 480GPa, when the temperature is increased to 900 ℃, the hardness value of 35.8GPa can still be maintained, and the elastic modulus is 497 GPa.
FIG. 5 shows Ti in examples 1 to 30.42Al0.47Cr0.11N、Ti0.34Al0.48Cr0.11Ta0.07N and Ti0.20Al0.20Cr0.20Ta0.20W0.20And (3) scanning electron microscope images of fracture sections of the N coating after constant temperature oxidation for 5 hours at 850 ℃ and 900 ℃. Ti at 850 DEG C0.34Al0.48Cr0.11Ta0.07N and Ti0.20Al0.20Cr0.20Ta0.20W0.20The oxidation resistance of the N coating is excellent, while the TiAlN coating in the comparative example 1 can be severely oxidized at 850 ℃; at 900 ℃ Ti0.42Al0.47Cr0.11N is completely oxidized, Ti0.34Al0.48Cr0.11Ta0.07The N coating is mostly oxidized, and Ti0.20Al0.20Cr0.20Ta0.20W0.20The N coating still keeps higher oxidation resistance, and the surface oxide has a compact structure and has a certain barrier effect on the internal diffusion of oxygen.
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 (9)
1. The multicomponent nitride hard coating is characterized by comprising a (TiAlCrTaW) N layer, wherein the (TiAlCrTaW) N layer is in a columnar crystal growth structure, and the chemical formula of the (TiAlCrTaW) N layer is (Ti)aAlbCrcTadWe) N, wherein a + b + c + d + e is 1; a is more than or equal to 0.2<0.5；0.2≤b<0.5；0<c≤0.2；0<d≤0.2；0<e≤0.2。
2. The multi-component nitride hard coating according to claim 1, wherein the hard coating has a hardness value of 30 to 40GPa and an elastic modulus of 400 to 500GPa in a deposited state.
3. The multi-component nitride hard coating according to claim 1, wherein the hard coating has a hardness value of 35 to 45GPa and an elastic modulus of 450 to 550GPa at 900 ℃.
4. The method for preparing a multi-component nitride hard coat according to any one of claims 1 to 3, comprising the following specific steps:
s1, putting the cleaned and dried substrate material into a PVD vacuum coating chamber, and vacuumizing to 1-6 multiplied by 10-3Pa；
S2, heating the cavity to 300-400 ℃, keeping the temperature constant, introducing Ar gas to adjust the air pressure of the cavity, and performing high-energy beam ion etching cleaning on the substrate;
s3, closing the Ar gas valve and introducing N2Adjusting the air pressure of the chamber, igniting the corresponding target by adopting a cathodic arc evaporation deposition method, setting the target current, setting the bias voltage to be-80 to-150V under the nitrogen atmosphere, and depositing (Ti)aAlbCrcTadWe) And N coating to obtain the multicomponent nitride hard coating.
5. The method of claim 4, wherein the substrate material in step S1 is WC-Co-TiC alloy, WC-Co alloy, WC-TiC-TaC (NbC) -Co alloy, or high speed steel.
6. The method for preparing a multi-component nitride hard coating according to claim 4, wherein the chamber pressure in step S2 is 0.5-1 Pa.
7. The method of claim 4, wherein in step S3, the chamber pressure is 2-4 Pa and the target current is 65-95A.
8. The method for preparing a multi-component nitride hard coating according to claim 4, wherein the deposition time in step S3 is 60-120 min.
9. Use of the multi-component nitride hard coating according to any one of claims 1 to 3 in the field of turning, milling and drilling.
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