CN109666887A - A kind of TiAlN hard coat and its preparation method and application - Google Patents

A kind of TiAlN hard coat and its preparation method and application Download PDF

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Publication number
CN109666887A
CN109666887A CN201811622631.1A CN201811622631A CN109666887A CN 109666887 A CN109666887 A CN 109666887A CN 201811622631 A CN201811622631 A CN 201811622631A CN 109666887 A CN109666887 A CN 109666887A
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hard coat
tialn
target
tialn hard
preparation
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CN109666887B (en
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王启民
彭滨
许雨翔
刘喆人
张权
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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
    • C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
    • C23C14/0641—Nitrides
    • 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
    • C23C14/22—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

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Physical Vapour Deposition (AREA)
  • Cutting Tools, Boring Holders, And Turrets (AREA)

Abstract

The invention belongs to coating material field, a kind of TiAlN hard coat and preparation method thereof is disclosed.This method carries out polishing ultrasonic cleaning to hard alloy substrate, then is put into coating machine chamber after drying up dedusting, and heating cavity is warming up to 400~600 DEG C, makes its vacuum degree 1~6 × 10‑3Pa is cooled to 300~400 DEG C and constant temperature；It is passed through Ar gas, bias is loaded to workpiece rotating frame, matrix surface aura is cleaned；Ar throughput is adjusted, cavity air pressure is controlled, Zr target is lighted using cathodic arc evaporation sedimentation, Zr target current and workpiece rotating frame bias are set, metal ion etching is carried out to matrix；It closes Ar air valve and is passed through N2, chamber pressure and workpiece rotating frame bias are adjusted, Ti is lighted50Al50Target simultaneously adjusts its electric current, in matrix surface depositing Ti AlN hard coat.The TiAlN hard coat has high thermal stability and basal body binding force.

Description

A kind of TiAlN hard coat and its preparation method and application
Technical field
The invention belongs to Materials Science and Engineering technical fields, more particularly, to a kind of TiAlN hard coat and its system Preparation Method and application.
Background technique
The fast development of advanced manufacturing technology (Ultra-precision Turning, High-speed machining etc.) make modern cutting technology constantly to High-precision, high efficiency, energy conservation and environmental protection direction it is fast-developing.Hard alloy as it is a kind of with refractory metal compound (WC, TiC, TaC etc.) it is matrix, with magnesium-yttrium-transition metal (Co, Fe, Ni etc.) for Binder Phase, pass through the cermet of powder metallurgy process preparation Type tool materials are favored, extensively because it is with excellent performances such as good intensity, hardness and wearabilities by modern cutting technology The general basis material as metal cutting tool.And pass through the technologies such as physical vapour deposition (PVD) (PVD), chemical vapor deposition (CVD) One layer of wear Protection coating (such as TiAlN hard coat) is coated on hard alloy cutter has become modern cutting tools development Important directions.
Hard coated cutting tool subjects high temperature load, hard in use (especially DRY CUTTING resist processing material) Binder Phase element (such as Co) can be preferentially diffused into surface covering in alloy base material, cause the premature failure of cutter.Metal Ion etching technology can be good at improving the film-substrate cohesion of hard alloy cutter coating, but for Co in high-speed dry type cutting Elements diffusion also lacks corresponding technical matters.
Summary of the invention
The object of the present invention is to provide a kind of preparation method of TiAlN hard coat, this method is steamed based on cathode arc Deposition technique and ion etching technology are sent out, by designing ion etch process, optimizes etch process parameters, it is hard to improve TiAlN The high high-temp stability of binding force and coating between matter coating and hard alloy substrate.
Another object of the present invention is to provide a kind of TiAlN hard coats of above method preparation.
A further object of the present invention is to provide a kind of applications of above-mentioned TiAlN hard coat.
The present invention is realized by following technical proposals:
A kind of preparation method of TiAlN hard coat, comprises the following specific steps that:
S1. matrix cleans: hard alloy substrate is processed by shot blasting, it is then clear using acetone and dehydrated alcohol ultrasonic wave It washes, then is packed into vacuum coating equipment chamber after drying up dedusting with general nitrogen；
S2. aura cleans: heating cavity is warming up to 400~600 DEG C, and is evacuated to vacuum degree 1.0~6.0 to cavity ×10-3Pa, vacuum are down to 300~400 DEG C and keep constant temperature；Ar gas is then passed to, cavity air pressure is adjusted, is turned to workpiece Frame loads bias, carries out aura cleaning to cemented carbide substrate surfaces；
S3. metal ion etches: control is passed through Ar throughput, cavity air pressure is adjusted, using cathodic arc evaporation sedimentation point Zr target is fired, Zr target current and workpiece rotating frame bias are set, metal ion etching is carried out to hard alloy substrate；
S4. it depositing Ti AlN hard coat: closes Ar air valve and is passed through N2, adjust chamber pressure and workpiece rotating frame bias, point Fire Ti50Al50Simultaneously its electric current progress coating deposition is arranged in target, and TiAlN hard coat is made in cemented carbide substrate surfaces, described The atom percentage content of each element in TiAlN hard coat are as follows: Ti:25~30at.%, Al:20~25at.%, N:48~ 52at.%.
Preferably, the time of cleaning described in step S1 is 40~60min.
Preferably, the flow of Ar gas described in step S2 is 200~300sccm, and the air pressure is 1.5~3.0Pa, described Workpiece rotating frame bias is -800~-1000V.
Preferably, the time of the cleaning of aura described in step S2 is 20~40min.
Preferably, the flow of Ar gas described in step S3 is 50~120sccm, and the cavity air pressure is 0.5~1.0Pa； The Zr target current is 80~110A, and the workpiece rotating frame bias is -800~-1000V, time of the etching is 2~ 20min。
Preferably, N described in step S42Flow be 200~400sccm, the air pressure of the chamber is 2.0~4.0Pa.
Preferably, Ti described in step S450Al50The purity of target is 99.95%, the Ti50Al50Target current be 70~ 100A, the workpiece rotating frame bias are -80~-200V, and the time of the deposition is 60~120min.
The TiAlN hard coat of above method preparation, the TiAlN hard coat are cubic structure, each element in coating Atom percentage content are as follows: Ti:25~30at.%, Al:20~25at.%, N:48~52at.%.
Preferably, the TiAlN hard coat with a thickness of 3~6 μm.
The TiAlN hard coat effectively overcomes influence of the high temperature lower substrate elements diffusion effect to coating performance, With good high-temperature stability and age-hardening effect, it can be used for the machining of the difficult-to-machine materials such as stainless steel.
The present invention is based on cathodic arc evaporation deposition techniques and ion etching technology, by designing ion etch process, optimization Procedure parameter realizes the promotion of TiAlN hard coat film-substrate cohesion and high high-temp stability.Technical process is as follows: first Hard alloy substrate is processed by shot blasting and ultrasonic cleaning, rear vacuum chamber of being sent into carry out aura cleaning, activation hard closes Golden matrix surface excites metal Zr ion etching cemented carbide substrate surfaces using cathodic arc evaporation deposition technique, changes hard The distribution of alloy substrate surface C o Binder Phase finally deposits the TiAlN hard of one layer of 3~6 μ m-thick in cemented carbide substrate surfaces Coating.The metal ion etching process of optimization significantly improves film-substrate cohesion under the premise of not introducing additional " drop " defect； The method of the present invention can form good Co element in cemented carbide substrate surfaces and preferentially etch phenomenon simultaneously, be formed Co layers poor, have Effect ground slows down the diffusion of Co under high temperature, so that the TiAlN hard coat on hard alloy substrate being capable of table at a high temperature of 900 DEG C Reveal typical age-hardening phenomenon, improve the mechanical performance and high high-temp stability of TiAlN hard coat, is further promoted The mechanical performance of the families of coatings, meets the needs of modern machining.
Compared with prior art, the invention has the following advantages:
1. method of the invention while guaranteeing TiAlN hard coat and basal body binding force, avoids additional " drop " Defect introduces, and obtains good coating surface quality.
2. the present invention can form good preferentially etching effect in cemented carbide substrate surfaces, Co under high temperature is slowed down Diffusion, so that the TiAlN hard coat on hard alloy substrate can still show typical age-hardening phenomenon, significantly mentions The high high high-temp stability of hard alloy cutter coating.
3. preparation method of the invention is simple, strong operability, controllability is good, is suitable for component of machine, knife mold etc. The protection of product surface has preferable economic benefit.
Detailed description of the invention
Fig. 1 is the structural schematic diagram of vacuum coating equipment cavity.
Fig. 2 is that Zr ion bombardment pre-processes and compares Cr ion bombardment in example 1~9, Ti ion bombardment in Examples 1 to 3 And Ti50Al50The secondary electron pattern of cemented carbide substrate surfaces after bombardment pretreatment.
Fig. 3 is to prepare TiAlN hard coat in embodiment 4 and compare the TiAlN hard coat table prepared in example 10~12 Face and section secondary electron pattern.
Fig. 4 is to prepare TiAlN hard coat in embodiment 4 and compare the XRD for preparing TiAlN hard coat in example 10~12 Map.
Fig. 5 is to prepare TiAlN hard coat in embodiment 4 and compare to prepare TiAlN hard coat in example 10~12 not Hardness after synthermal lower vacuum annealing 30 minutes.
Specific embodiment
The contents of the present invention are further illustrated combined with specific embodiments below, but should not be construed as limiting the invention. Unless otherwise specified, the conventional means that technological means used in embodiment is well known to those skilled in the art.Except non-specifically Illustrate, reagent that the present invention uses, method and apparatus is the art conventional reagents, method and apparatus.
Embodiment 1
PVD vacuum coating equipment A1 target position fills Zr target.Hard alloy substrate (WC-8wt.%Co-4wt.%TiC) is thrown Light processing is packed on vacuum chamber charging tray after being dried up with general nitrogen by acetone, dehydrated alcohol ultrasonic cleaning 60min.It opens and adds Hot device is warming up to 500 DEG C, and heating process opens vacuum system, is evacuated to vacuum degree 5.0 × 10 to chamber-3Pa or less.Setting Temperature is 350 DEG C, and being passed through Ar throughput is 300sccm, and control chamber pressure is 2.0Pa, and setting workpiece rotating frame bias is -800V, right Hard alloy substrate carries out aura cleaning, and aura scavenging period is 30min.Adjusting Ar throughput is 70sccm, and control chamber pressure is 0.55Pa, holding workpiece rotating frame bias are -800V, light Zr target, target current 105A, ion etching continues the short period. After completing ion etching, target power supply and gas valve are closed, is down to room temperature to vacuum chamber temperature, vacuum chamber is opened and takes out Hard alloy substrate.
Fig. 1 is vacuum coating equipment cavity body structure schematic diagram.From fig. 1, it can be seen that two target position of A1 and A2 are distributed on the left of cavity, it is right Side is distributed two target position of B1 and B2；Aura cleaning, ion etching process and the revolution operation of coating process transfer rack, charging tray are transported certainly Row；It is plasma atmosphere in cavity in technical process.
Embodiment 2
PVD vacuum coating equipment A1 target position fills Zr target.Hard alloy substrate (WC-8wt.%Co-4wt.%TiC) is thrown Light processing is packed on vacuum chamber charging tray after being dried up with general nitrogen by acetone, dehydrated alcohol ultrasonic cleaning 60min.It opens and adds Hot device is warming up to 500 DEG C, and heating process opens vacuum system, is evacuated to vacuum degree 5.0 × 10 to chamber-3Pa or less.Setting Temperature is 350 DEG C, and being passed through Ar throughput is 300sccm, and control chamber pressure is 2.0Pa, and setting workpiece rotating frame bias is -800V, right Hard alloy substrate carries out aura cleaning, and aura scavenging period is 30min.Adjusting Ar throughput is 70sccm, and control chamber pressure is 0.55Pa, holding workpiece rotating frame bias are -800V, light Zr target, target current 105A, ion etching continues medium while. After completing ion etching, target power supply and gas valve are closed, is down to room temperature to vacuum chamber temperature, vacuum chamber is opened and takes out Hard alloy substrate.
Embodiment 3
PVD vacuum coating equipment A1 target position fills Zr target.Hard alloy substrate (WC-8wt.%Co-4wt.%TiC) is thrown Light processing is packed on vacuum chamber charging tray after being dried up with general nitrogen by acetone, dehydrated alcohol ultrasonic cleaning 60min.It opens and adds Hot device is warming up to 500 DEG C, and heating process opens vacuum system, is evacuated to vacuum degree 5.0 × 10 to chamber-3Pa or less.Setting Temperature is 350 DEG C, and being passed through Ar throughput is 300sccm, and control chamber pressure is 2.0Pa, and setting workpiece rotating frame bias is -800V, right Hard alloy substrate carries out aura cleaning, and aura scavenging period is 30min.Adjusting Ar throughput is 70sccm, and control chamber pressure is 0.55Pa, holding workpiece rotating frame bias are -800V, light Zr target, target current 105A, ion etching last longer. After completing ion etching, target power supply and gas valve are closed, is down to room temperature to vacuum chamber temperature, vacuum chamber is opened and takes out Hard alloy substrate.
Compare example 1
With in embodiment 1 the difference is that: the A1 target position fills Cr target；Target current is 100A.Compare example 2
With in embodiment 1 the difference is that: the A1 target position fills Ti target；Target current is 100A.Compare example 3
With in embodiment 1 the difference is that: the A1 target position fills Ti50Al50Target；Target current is 80A.Compare example 4
With in embodiment 2 the difference is that: the A1 target position fills Cr target；Target current is 100A.Compare example 5
With in embodiment 2 the difference is that: the A1 target position fills Ti target；Target current is 100A.Compare example 6
With in embodiment 2 the difference is that: the A1 target position fills Ti50Al50Target；Target current is 80A.Compare example 7
With in embodiment 3 the difference is that: the A1 target position fills Cr target；Target current is 100A.Compare example 8
With in embodiment 3 the difference is that: the A1 target position fills Ti target；Target current is 100A.Compare example 9
With in embodiment 3 the difference is that: the A1 target position fills Ti50Al50Target；Target current is 80A.
Fig. 2 is Examples 1 to 3 and the secondary electron pattern for comparing matrix surface after different pretreatments technique in example 1~9 Figure.Examples 1 to 3 and comparison example 1~9 proceed to ion-etching step (preprocessing part), apply without depositing Ti AlN hard Layer.Comparison finds that cemented carbide substrate surfaces show apparent Co Binder Phase and preferentially etch phenomenon in the present invention, while without bright The introducing of aobvious bulky grain.
Embodiment 4
PVD vacuum coating equipment A1 target position fills Zr target, and B1 target position fills Ti50Al50Target.By hard alloy substrate (WC-8wt.% Co-4wt.%TiC it) is processed by shot blasting, is packed by acetone, dehydrated alcohol ultrasonic cleaning 60min, after being dried up with general nitrogen true On plenum chamber charging tray.It opens heater and is warming up to 500 DEG C, heating process opens vacuum system, is evacuated to vacuum degree to chamber 5.0×10-3Pa or less.It is 350 DEG C that temperature, which is arranged, and being passed through Ar throughput is 300sccm, and control chamber pressure is 2.0Pa, and workpiece is arranged Pivoted frame bias is -800V, carries out aura cleaning to hard alloy substrate, aura scavenging period is 30min.Adjusting Ar throughput is 70sccm, control chamber pressure are 0.55Pa, and holding workpiece rotating frame bias is -800V, light Zr target, target current 105A, ion Etch last longer.Zr target and Ar air valve are closed, N is passed through2Gas velocity is 300sccm, and control chamber pressure is 3.0Pa.It adjusts Section workpiece rotating frame bias is -100V, lights Ti50Al50Target, setting target current are 80A, 90min are deposited, in carbide matrix Body surface wheat flour is for TiAlN hard coat.
The atom percentage content of each element in the TiAlN hard coat are as follows: Ti:27at.%, Al:23at.%, N: 50at.%.The TiAlN hard coat with a thickness of 5.8 μm.After completing plated film, target power supply and gas valve are closed, to true Cavity room temperature is down to room temperature, opens vacuum chamber and takes out plated film matrix.
Embodiment 5
With in embodiment 4 the difference is that: the atom percentage content of each element in the TiAlN hard coat are as follows: Ti:25at.%, Al:25at.%, N:50at.%.The TiAlN hard coat with a thickness of 3 μm.
Embodiment 6
With in embodiment 4 the difference is that: the atom percentage content of each element in the TiAlN hard coat are as follows: Ti:30at.%, Al:22at.%, N:48at.%.The TiAlN hard coat with a thickness of 4 μm.
Embodiment 7
With in embodiment 4 the difference is that: the atom percentage content of each element in the TiAlN hard coat are as follows: Ti:28at.%, Al:20at.%, N:52at.%.The TiAlN hard coat with a thickness of 5 μm.
Embodiment 8
With in embodiment 4 the difference is that: the atom percentage content of each element in the TiAlN hard coat are as follows: Ti:25at.%, Al:24at.%, N:51at.%.The TiAlN hard coat with a thickness of 6 μm.
Embodiment 9
With in embodiment 4 the difference is that: the atom percentage content of each element in the TiAlN hard coat are as follows: Ti:28at.%, Al:22at.%, N:50at.%.The TiAlN hard coat with a thickness of 4 μm.Compare example 10
PVD vacuum coating equipment B1 target position fills Ti50Al50Target.By hard alloy substrate (WC-8wt.%Co-4wt.%TiC) It is processed by shot blasting, by acetone, dehydrated alcohol ultrasonic cleaning 60min, is packed on vacuum chamber charging tray after being dried up with general nitrogen. It opens heater and is warming up to 500 DEG C, heating process opens vacuum system, is evacuated to vacuum degree 5.0 × 10 to chamber-3Pa with Under.Be arranged temperature be 350 DEG C, be passed through Ar throughput be 300sccm, control chamber pressure be 2.0Pa, setting workpiece rotating frame bias be- 800V carries out aura cleaning to hard alloy substrate, and aura scavenging period is 30min.Ar air valve is closed, N is passed through2Gas velocity For 300sccm, control chamber pressure is 3.0Pa.Adjusting workpiece rotating frame bias is -100V, lights Ti50Al50Target current is arranged in target For 80A, 90min is deposited, prepares TiAlN hard coat in cemented carbide substrate surfaces.Each element in the TiAlN hard coat Atom percentage content are as follows: Ti:28at.%, Al:23at.%, N:49at.%.Complete plated film after, close target power supply and Gas valve is down to room temperature to vacuum chamber temperature, opens vacuum chamber and takes out plated film matrix.
Compare example 11
With in embodiment 4 the difference is that: the A1 target position fills Cr target；The target current is 100A；The TiAlN The atom percentage content of each element in hard coat are as follows: Ti:28at.%, Al:21at.%, N:51at.% ".
Compare example 12
With in embodiment 4 the difference is that: the A1 target position fills Ti target；The adjusting Ar throughput is 140sccm, control Chamber pressure processed is 0.50Pa, and holding workpiece rotating frame bias is -100V, lights Ti target, target current 100A, sedimentation time 10min； The closing Zr target and Ar air valve are as follows: close Ti target and control N2Flow；The atom of each element in the TiAlN hard coat Degree are as follows: Ti:26at.%, Al:24at.%, N:50at.% ".
Fig. 3 is embodiment 4 and compares the TiAlN hard coat surface prepared in example 10~12 and section secondary electron pattern Figure.Comparison finds that coating prepared by the present invention shows fine and close columnar crystal structure, and coating surface is without obvious bulky grain.Fig. 4 It is embodiment 4 with the TiAlN hard coat glancing incidence XRD spectrum prepared in comparison example 10~12.Comparison discovery, the present invention are made Standby coating surface goes out apparent (111) direction texture.
To embodiment 4 and compare the TiAlN hard coat progress vacuum heat treatment experiment prepared in example 10~12, Vacuum Heat Processing experiment carries out in high-temperature vacuum annealing furnace, and chamber vacuum degree is 5.0 × 10-3Pa, selecting heat treatment temperature is respectively 800 DEG C, 900 DEG C, 1000 DEG C, 1100 DEG C, 1200 DEG C, heating rate 10K/min, soaking time 30min take furnace cooling Mode.Fig. 5 is TiAlN hard coat and compare the TiAlN hard coat prepared in example 10~12 in difference prepared by embodiment 4 At a temperature of anneal 30min after hardness (compare example 10 in TiAlN hard coat 1000 and 1100 DEG C annealing after peel off). Comparison discovery, TiAlN hard coat prepared by the present invention can still show typical age-hardening phenomenon at high temperature The nano-size domain of rich Ti and richness Al (TiAlN spinodal decomposition at).
The above embodiment is a preferred embodiment of the present invention, but embodiments of the present invention are not by above-described embodiment Limitation, it is other it is any without departing from the spirit and principles of the present invention made by change, modification, substitution, combination and simplify, It should be equivalent substitute mode, be included within the scope of the present invention.

Claims (10)

1. a kind of preparation method of TiAlN hard coat, which is characterized in that comprise the following specific steps that:
S1. matrix cleans: hard alloy substrate is processed by shot blasting, acetone and dehydrated alcohol ultrasonic cleaning are then used, It is packed into vacuum coating equipment chamber after drying up dedusting with general nitrogen again；
S2. aura cleans: heating cavity is warming up to 400~600 DEG C, and is evacuated to vacuum degree 1.0~6.0 × 10 to cavity-3Pa, vacuum are down to 300~400 DEG C and keep constant temperature；Then pass to Ar gas, adjust cavity air pressure, to workpiece rotating frame plus Bias is carried, aura cleaning is carried out to cemented carbide substrate surfaces；
S3. metal ion etches: control is passed through Ar throughput, adjusts cavity air pressure, lights Zr using cathodic arc evaporation sedimentation Zr target current and workpiece rotating frame bias is arranged in target, carries out metal ion etching to hard alloy substrate；
S4. it depositing Ti AlN hard coat: closes Ar air valve and is passed through N2, chamber pressure and workpiece rotating frame bias are adjusted, is lighted Ti50Al50Simultaneously its electric current progress coating deposition is arranged in target, and TiAlN hard coat is made in cemented carbide substrate surfaces, described The atom percentage content of each element in TiAlN hard coat are as follows: Ti:25~30at.%, Al:20~25at.%, N:48~ 52at.%.
2. the preparation method of TiAlN hard coat according to claim 1, which is characterized in that cleaned described in step S1 Time be 40~60min.
3. the preparation method of TiAlN hard coat according to claim 1, which is characterized in that Ar gas described in step S2 Flow be 200~300sccm, the air pressure be 1.5~3.0Pa, the workpiece rotating frame bias be -800~-1000V.
4. the preparation method of TiAlN hard coat according to claim 1, which is characterized in that aura described in step S2 The time of cleaning is 20~40min.
5. the preparation method of TiAlN hard coat according to claim 1, which is characterized in that Ar gas described in step S3 Flow be 50~120sccm, the cavity air pressure be 0.5~1.0Pa；The Zr target current is 80~110A, the workpiece Pivoted frame bias is -800~-1000V, and the time of the etching is 2~20min.
6. the preparation method of TiAlN hard coat according to claim 1, which is characterized in that N described in step S42Stream Amount is 200~400sccm, and the air pressure of the chamber is 2.0~4.0Pa.
7. the preparation method of TiAlN hard coat according to claim 1, which is characterized in that described in step S4 Ti50Al50The purity of target is 99.95%, the Ti50Al50Target current be 70~100A, the workpiece rotating frame bias be -80~- 200V, the time of the deposition are 60~120min.
8. the TiAlN hard coat of method preparation according to claim 1-7, which is characterized in that the TiAlN Hard coat is cubic structure, the atom percentage content of each element in coating are as follows: Ti:25~30at.%, Al:20~ 25at.%, N:48~52at.%.
9. TiAlN hard coat according to claim 8, which is characterized in that the TiAlN hard coat with a thickness of 3 ~6 μm.
10. application of the TiAlN hard coat in the cutting tool of processing stainless steel material described in claim 8 or 9.
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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110484870A (en) * 2019-08-15 2019-11-22 广东工业大学 A kind of multicomponent nitride hard coating and its preparation method and application
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