CN108950488A - TiAl/TiAlN/TiZrAlN composite coating and preparation method thereof - Google Patents

TiAl/TiAlN/TiZrAlN composite coating and preparation method thereof Download PDF

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CN108950488A
CN108950488A CN201810875578.XA CN201810875578A CN108950488A CN 108950488 A CN108950488 A CN 108950488A CN 201810875578 A CN201810875578 A CN 201810875578A CN 108950488 A CN108950488 A CN 108950488A
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tialn
tial
metallic matrix
titanium
time
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王建民
高术振
李阳
张钧
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Hebei University of Engineering
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Hebei University of Engineering
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    • CCHEMISTRY; METALLURGY
    • C23COATING 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
    • C23CCOATING 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
    • C23C14/00Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/22Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
    • C23C14/24Vacuum evaporation
    • C23C14/32Vacuum evaporation by explosion; by evaporation and subsequent ionisation of the vapours, e.g. ion-plating
    • C23C14/325Electric arc evaporation
    • CCHEMISTRY; METALLURGY
    • C23COATING 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
    • C23CCOATING 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
    • C23C14/00Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/0021Reactive sputtering or evaporation
    • CCHEMISTRY; METALLURGY
    • C23COATING 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
    • C23CCOATING 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
    • C23C14/00Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/06Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
    • C23C14/0641Nitrides
    • CCHEMISTRY; METALLURGY
    • C23COATING 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
    • C23CCOATING 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
    • C23C14/00Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/06Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
    • C23C14/14Metallic material, boron or silicon
    • C23C14/16Metallic material, boron or silicon on metallic substrates or on substrates of boron or silicon

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  • Engineering & Computer Science (AREA)
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Abstract

The present invention provides a kind of TiAl/TiAlN/TiZrAlN composite coating and preparation method thereof, method includes: to select the titanium-aluminum alloy target that two Ti/Al atomic ratios are 50/50 and the titanium-zirconium alloy target that two Ti/Zr atomic ratios are 45/55;Metallic matrix is placed on work rest;Pre-firing processes are carried out to coating chamber;Pre- Bombardment and cleaning technique is carried out to metallic matrix;TiAl layers are plated on metallic matrix;TiAlN layers are plated on TiAl layer;TiZrAlN layers are plated on TiAlN layer.The TiAl/TiAlN/TiZrAlN composite coating that the present invention obtains can reach superhard, while realization while also ensure high adhesion force and highly heatproof and shockproof, reduce film layer internal stress, and with good stability.

Description

TiAl/TiAlN/TiZrAlN composite coating and preparation method thereof
Technical field
The present invention relates to TiAl/TiAlN/TiZrAlN composite coatings and preparation method thereof.
Background technique
There are some defects to easily lead to when in use such as the poor adhesive force between coating and matrix for existing composite coating Coating edge residual thermal stress is excessive, it is cracked so as to cause coating, peel off phenomena such as;And between different coating and matrix Changes in material properties transition is big, is easy to further result in stress concentration, hardness is inadequate, and stability is poor.
Summary of the invention
The object of the present invention is to provide a kind of preparation method of the superhard composite coating of TiAl/TiAlN/TiZrAlN, this method Realization while ensure that film layer can reach superhard, while also ensuring high adhesion force and highly heatproof and shockproof, reduces film layer Internal stress, and it is with good stability.
The present invention provides a kind of methods for preparing TiAl/TiAlN/TiZrAlN composite coating, comprising: selects two Ti/ The titanium-zirconium alloy target that the titanium-aluminum alloy target and two Ti/Zr atomic ratios that Al atomic ratio is 50/50 are 45/55;By gold to be coated Belong to matrix to be placed on the work rest of coating chamber;Pre-firing processes are carried out to the coating chamber;It is clear that pre- bombardment is carried out to metallic matrix Wash technique;TiAl layers are plated on the metallic matrix, arcing time is at the first time;TiAlN layers are plated on the TiAl layer, are risen The arc time was the second time;TiZrAlN layers are plated on the TiAlN layer, arcing time is the third time;Wherein, described first The ratio of time, second time and the third time are 1:3:6.
In the above-mentioned methods, wherein the titanium-aluminum alloy target that two Ti/Al atomic ratios are 50/50 is in the coating chamber 90 degree of configurations, the titanium-zirconium alloy target that two Ti/Zr atomic ratios are 45/55 is in the coating chamber in 90 degree of configurations.
In the above-mentioned methods, wherein the metallic matrix is high-speed steel or hard alloy, and by gold to be coated Before category matrix is placed on the work rest of coating chamber, the metallic matrix is carried out at decontamination, polishing, ultrasonic cleaning and drying Reason.
In the above-mentioned methods, wherein the film surface to be plated of the metallic matrix and titanium-aluminum alloy target and titanium-zirconium alloy target The distance on surface is in 25-30cm.
In the above-mentioned methods, wherein carrying out pre-firing processes to the coating chamber includes: the vacuum degree in the coating chamber Reach 3 × 10-2When pa, starting baking electric current, the temperature of the coating chamber reach 200 DEG C used in the time not less than 20 minutes.
In the above-mentioned methods, wherein carrying out pre- Bombardment and cleaning technique to each alloys target includes: the back when the coating chamber Bottom vacuum degree reaches 8.0 × 10-3Pa, prebake conditions temperature are filled with argon gas when reaching 200 DEG C, reach the pressure of the coating chamber 2.2×10-1Pa~2.8 × 10-1Pa opens each alloys target arc source, and arc current is kept to stablize between 55~60 amperes, into Row ion bombardment 15 minutes, bias was bombarded from 350 volts and progressively increases to 400 volts.
In the above-mentioned methods, wherein plating TiAl layers on the metallic matrix includes: by the indoor Ar Pressure of the plated film It is maintained at 2.2 × 10 by force-1Pa~2.8 × 10-1Pa, the arc current of two titanium-aluminum alloy targets are placed between 55~60 amperes, institute The back bias voltage for stating metallic matrix is set as -220 volts, and the first time is no more than 10 minutes.
In the above-mentioned methods, wherein it is 0 that TiAlN layers of plating, which includes: adjusting ar pressure, on the TiAl layer, makes nitrogen Pressure reaches 2.6 × 10-1Pa~2.8 × 10-1Pa, the arc current of two titanium-aluminum alloy targets are placed between 55~60 amperes, institute The back bias voltage for stating metallic matrix is set as -200 volts.
In the above-mentioned methods, wherein plating TiZrAlN layers on the TiAlN layer includes: by the indoor nitrogen of the plated film Pressure is maintained at 2.8 × 10-1The arc current of pa, two titanium-aluminum alloy targets and two titanium-zirconium alloy targets is placed in 60-62 ampere Between, the back bias voltage of the metallic matrix is set as -180 volts.
The present invention also provides the TiAl/TiAlN/TiZrAlN composite coatings prepared by the above method.
The TiAl/TiAlN/TiZrAlN composite coating that the present invention obtains can reach superhard, while also ensure high attached Put forth effort to reduce film layer internal stress, and with good stability with realization while highly heatproof and shockproof.
Specific embodiment
The following examples can make those skilled in the art that the present invention be more fully understood, but not limit in any way The present invention.
The present invention provides a kind of preparation methods of the superhard composite coating of TiAl/TiAlN/TiZrAlN, including with lower section Face:
1, the determination of deposition technique: system of the multi-arc ion coating as the superhard composite coating of TiAl/TiAlN/TiZrAlN is determined Standby technology.
2, the determination of arc source target: determine that 2 Ti/Al atomic ratios are 50/50 titanium-aluminum alloy target and 2 Ti/Zr atoms Than the titanium-zirconium alloy target for 45/55 combination as plated film arc source target.
3, the determination of arc source number: requiring according to membrane uniformity and the temperature limiting of metallic matrix to be coated is to determine Multi-arc ion coating arc to be used source number, that is, to guarantee membrane uniformity, at least according to the combination in method and step 2 The arc source starting the arc simultaneously selecting two different height different directions and being configured at 90 degree, and to guarantee metallic matrix to be coated simultaneously During the entire process of coating chamber, plated film room temperature is no more than the temperature that matrix allows.
4, metallic matrix to be coated select and pre-treatment: select high-speed steel or hard alloy as Metal Substrate to be coated Body carries out it using metal detergent conventional deoil, decontamination processing and carry out surface throwing before being put into coating chamber and carrying out plated film Light processing finally carries out ultrasonic cleaning with acetone and ethyl alcohol respectively, and hair dryer drying is subsequently placed in the work of coating chamber with spare On part frame.
5, metallic matrix film surface to be plated is to the linear distance of target material surface in 25-30cm.
6, the determination of pre-firing processes: refer to for the acquisition superhard composite coating of TiAl/TiAlN/TiZrAlN and in ion bombardment The heated baking technique that technique carries out before starting, reaches 3 × 10 in coating chamber vacuum degree-2When pa, starting baking electric current, to keep away Exempt from thermal stress accumulation, toasted using (60-100 amperes) of low current, and keep the work rest uniform rotation of bearing metal matrix, is plated Film room temperature reach 200 DEG C used in the time not less than 20 minutes.
7, the determination of pre- Bombardment and cleaning technique: refer to for the acquisition superhard composite coating of TiAl/TiAlN/TiZrAlN and in plating The ion bombardment technique carried out before titanium-aluminium alloy transition zone, when coating chamber back end vacuum degree reaches 8.0 × 10-3Pa, prebake conditions Temperature is filled with argon gas when reaching 200 DEG C, and plated film chamber pressure is made to reach 2.2 × 10-1Pa~2.8 × 10-1Pa opens each arc source, The restrictive condition for allowing temperature according to arc source target size size and matrix, keeps arc current to stablize between 55~60 amperes Some current value carries out ion bombardment 15 minutes, bombards bias from 350 volts and progressively increases to 400 volts.
8, the determination of sedimentation time: refer to for the acquisition superhard composite coating of TiAl/TiAlN/TiZrAlN and when the deposition of determination Between, entire deposition is determined according to the number in used multi-arc ion coating arc source and to (2.5-3 microns) requirements of thickness of film layer Then entire sedimentation time is divided into 1/3/6 by the time, wherein the sedimentation time of TiAl transition zone is the time of entire deposition process 10%, TiAlN middle layer sedimentation time be entire deposition process time 30%, outermost layer TiZrAlN film layer it is heavy The product time is the 60% of the time of entire deposition process.
9, the indoor ar pressure of plated film the determination of the preparation process of TiAl transition zone: is maintained at 2.2 × 10-1Pa~ 2.8×10-1Pa, the arc current of 2 titanium-aluminum alloy targets are placed in some current value between 55~60 amperes, metallic matrix negative bias Pressure is set as -220 volts, and arcing time is the 10% of the time of entire deposition process, and is no more than 10 minutes, then adjusts argon Air pressure is 0 by force, and nitrogen pressure reaches 2.6 × 10-1Pa~2.8 × 10-1It is superhard to be ready for TiAl/TiAlN/TiZrAlN for pa The deposition of the TiAlN middle layer of composite coating.
10, the indoor nitrogen pressure of plated film the determination of the preparation process of TiAlN middle layer: is maintained at 2.6 × 10-1Pa~ 2.8×10-1Pa, the arc current of 2 titanium-aluminum alloy targets are placed in some current value between 55~60 amperes, metallic matrix negative bias Pressure is set as -200 volts, and arcing time is the 30% of the time of entire deposition process.Then keeping or adjust nitrogen pressure is 2.6 ×10-1Pa is ready for the deposition of the outermost layer TiZrAlN film layer of the superhard composite coating of TiAl/TiAlN/TiZrAlN.
11, the determination of the preparation process of outermost layer TiZrAlN film layer: the indoor nitrogen pressure of plated film is maintained at 2.6 × 10-1The arc current of pa, 2 titanium-aluminum alloy targets and 2 titanium-zirconium alloy targets is placed between 60-62 amperes, metallic matrix back bias voltage - 180 volts are set as, arcing time is the 60% of the time of entire deposition process.
12, the control of plated film room temperature: refer to obtain the plating of TiAl/TiAlN/TiZrAlN superhard composite film layer and determination The limitation of film room temperature, for high speed steel substrate, plated film room temperature is no more than 380 degrees Celsius;For hard alloy substrate, plated film Room temperature is no more than 420 degrees Celsius.
13, work rest rotates: in coating chamber slow heating baking, carrying out ion bombardment, plating TiAl mistake to metallic matrix It crosses during the entire process of layer, TiAlN middle layer and outermost layer TiZrAlN film layer and is always maintained at work rest rotation, revolving speed 6 Rev/min.
According to the preparation method of the superhard composite coating of TiAl/TiAlN/TiZrAlN proposed by the invention, can obtain The superhard composite coating of the TiAl/TiAlN/TiZrAlN stated, due to using the control respectively of arc source alloy target current, Neng Goushi Existing membranous layer ingredient optimization, Ti/Al/Cr substantially remains in 2:1:1, to ensure that superhard composite coating can reach superhard; Simultaneously as being also ensured high attached using the film layer composition of multi-level progressive structure and the reasonable distribution of each layer sedimentation time Put forth effort to reduce film layer internal stress, and with good stability with realization while highly heatproof and shockproof.
It is illustrated below with reference to specific embodiment.
Embodiment 1
The superhard composite coating of TiAl/TiAlN/TiZrAlN is prepared on commercial high speed steel W18Cr4V.
1, the determination of deposition technique: system of the multi-arc ion coating as the superhard composite coating of TiAl/TiAlN/TiZrAlN is determined Standby technology.
2, the determination of arc source target: determine that 2 Ti/Al atomic ratios are 50/50 titanium-aluminum alloy target and 2 Ti/Zr atoms Than the titanium-zirconium alloy target for 45/55 combination as plated film arc source target.
3, the determination of arc source number: requiring according to membrane uniformity and the temperature limiting of metallic matrix to be coated is to determine Multi-arc ion coating arc to be used source number, that is, to guarantee membrane uniformity, selected according to the combination in method and step 2 Two different height different directions and the arc source configured at 90 degree the starting the arc simultaneously, and to guarantee that metallic matrix to be coated is plating simultaneously During the entire process of film room, plated film room temperature is no more than the temperature that metallic matrix allows.
4, metallic matrix to be coated select and pre-treatment: select high-speed steel as metallic matrix to be coated, be put into plating Before film room carries out plated film, it is carried out using metal detergent it is conventional deoil, decontamination processing and carry out surface polishing treatment, finally Ultrasonic cleaning is carried out with acetone and ethyl alcohol respectively, and hair dryer drying is subsequently placed on the work rest of coating chamber with spare.
5, high speed steel substrate coated surface is to the linear distance of target material surface in 25cm.
6, the determination of pre-firing processes: refer to for the acquisition superhard composite coating of TiAl/TiAlN/TiZrAlN and in ion bombardment The heated baking technique that technique carries out before starting, reaches 3 × 10 in coating chamber vacuum degree-2When pa, starting baking electric current, to keep away Exempt from thermal stress accumulation, using low current (60 amperes 10 minutes, 80 amperes 10 minutes, then improve baking electric current to 100 amperes) Baking, and keep carrying high speed steel substrate work rest uniform rotation, plated film room temperature reach 200 DEG C used in the time 42 divide Clock.
7, the determination of pre- Bombardment and cleaning technique: refer to for the acquisition superhard composite coating of TiAl/TiAlN/TiZrAlN and in plating The ion bombardment technique carried out before titanium-aluminium alloy transition zone, when coating chamber back end vacuum degree reaches 8.0 × 10-3Pa, prebake conditions Temperature is filled with argon gas when reaching 200 DEG C, and plated film chamber pressure is made to reach 2.5 × 10-1Pa opens each arc source, according to arc source target Size and high speed steel substrate allow the restrictive condition of temperature, keep arc current to stablize at 58 amperes, carry out ion bombardment 15 Minute, that is, 350 volts of bias of bombardment are kept for 5 minutes, and 380 volts are kept for 5 minutes, are then increased to 400 volts and are kept for 5 minutes.
8, the determination of sedimentation time: refer to for the acquisition superhard composite coating of TiAl/TiAlN/TiZrAlN and when the deposition of determination Between, according to the number in used multi-arc ion coating arc source and to thickness (the being preset as 2.8 microns) requirement of film layer, determine entire Sedimentation time 60 minutes, entire sedimentation time is then divided into 1/3/6, wherein the sedimentation time of TiAl transition zone is entire deposition The sedimentation time of 10%, the TiAlN middle layer of the time of process is the 30% of the time of entire deposition process, outermost layer The sedimentation time of TiCrAlN film layer is the 60% of the time of entire deposition process.
9, the indoor ar pressure of plated film the determination of the preparation process of TiAl transition zone: is maintained at 2.2 × 10-1Pa, 2 The arc current of titanium-aluminum alloy target is placed in 58 amperes, and high speed steel substrate back bias voltage is -220 volts, and arcing time is entirely to deposit The 10% of the time of journey, that is, 6 minutes, then adjusting ar pressure was 0, and nitrogen pressure reaches 2.6 × 10-1Pa is ready for The deposition of the TiAlN middle layer of the superhard composite coating of TiAl/TiAlN/TiZrAlN.
10, the indoor nitrogen pressure of plated film the determination of the preparation process of TiAlN middle layer: is maintained at 2.6 × 10-1Pa, 2 The arc current of a titanium-aluminum alloy target is placed in 58 amperes, and high speed steel substrate back bias voltage is -200 volts, and arcing time is entire deposition The 30% of the time of process, i.e., 18 minutes.Then keeping nitrogen pressure is 2.6 × 10-1Pa is ready for TiAl/TiAlN/ The deposition of the outermost layer TiZrAlN film layer of the superhard composite coating of TiZrAlN.
11, the determination of the preparation process of outermost layer TiZrAlN film layer: the indoor nitrogen pressure of plated film is maintained at 2.6 × 10-1The arc current of pa, 2 titanium-aluminum alloy targets and 2 titanium-zirconium alloy targets is placed in 62 amperes, and high speed steel substrate back bias voltage is -180 Volt, arcing time are the 60% of the time of entire deposition process, that is, 36 minutes.
12, the control of plated film room temperature: refer to obtain the plating of TiAl/TiAlN/TiZrAlN superhard composite film layer and determination The limitation of film room temperature, after high speed steel substrate completes entire coating process, plated film room temperature is 332 degrees Celsius;
13, work rest rotates: in coating chamber slow heating baking, carrying out ion bombardment, plating TiAl to high speed steel substrate Work rest rotation, revolving speed 6 are always maintained at during the entire process of transition zone, TiAlN middle layer and outermost layer TiZrAlN film layer Rev/min.
The superhard composite coating of TiAl/TiAlN/TiCrAlN for using the above method to prepare is measured, coating layer thickness It is 2.82 microns, using microhardness testers, under 25g power load, the hardness for measuring the superhard composite coating reaches 4200HV.
Embodiment 2
The superhard composite coating of TiAl/TiAlN/TiZrAlN is prepared on hard alloy YT15 matrix.
1, the determination of deposition technique: system of the multi-arc ion coating as the superhard composite coating of TiAl/TiAlN/TiZrAlN is determined Standby technology.
2, the determination of arc source target: determine that 2 Ti/Al atomic ratios are 50/50 titanium-aluminum alloy target and 2 Ti/Zr atoms Than the titanium-zirconium alloy target for 45/55 combination as plated film arc source target.
3, the determination of arc source number: requiring according to membrane uniformity and the temperature limiting of metallic matrix to be coated is to determine Multi-arc ion coating arc to be used source number, that is, to guarantee membrane uniformity, selected according to the combination in method and step 2 Two different height different directions and the arc source configured at 90 degree the starting the arc simultaneously, and to guarantee that metallic matrix to be coated is plating simultaneously During the entire process of film room, plated film room temperature is no more than the temperature that metallic matrix allows.
4, metallic matrix to be coated select and pre-treatment: select hard alloy YT15 as metallic matrix to be coated, It is put into before coating chamber carries out plated film, it is carried out using metal detergent conventional to deoil, decontamination processing and carry out at surface polishing Reason finally carries out ultrasonic cleaning with acetone and ethyl alcohol respectively, and hair dryer is dried up with spare, is subsequently placed in the work rest of coating chamber On.
5, substrate coated surface is to the linear distance of target material surface in 28cm.
6, the determination of pre-firing processes: refer to for the acquisition superhard composite coating of TiAl/TiAlN/TiZrAlN and in ion bombardment The heated baking technique that technique carries out before starting, reaches 3 × 10 in coating chamber vacuum degree-2When pa, starting baking electric current, to keep away Exempt from thermal stress accumulation, using low current (60 amperes 10 minutes, 80 amperes 10 minutes, then improve baking electric current to 100 amperes) Baking, and keep carrying hard alloy substrate work rest uniform rotation, plated film room temperature reach 200 DEG C used in the time 42 divide Clock.
7, the determination of pre- Bombardment and cleaning technique: refer to for the acquisition superhard composite coating of TiAl/TiAlN/TiZrAlN and in plating The ion bombardment technique carried out before titanium-aluminium alloy transition zone, when coating chamber back end vacuum degree reaches 8.0 × 10-3Pa, prebake conditions Temperature is filled with argon gas when reaching 200 DEG C, and plated film chamber pressure is made to reach 2.5 × 10-1Pa opens each arc source, according to arc source target Size and hard alloy substrate allow the restrictive condition of temperature, keep arc current to stablize at 58 amperes, carry out ion bombardment 15 minutes, that is, 350 volts of bias of bombardment are kept for 5 minutes, and 380 volts are kept for 5 minutes, are then increased to 400 volts and are kept for 5 minutes.
8, the determination of sedimentation time: refer to for the acquisition superhard composite coating of TiAl/TiAlN/TiZrAlN and when the deposition of determination Between, according to the number in used multi-arc ion coating arc source and to thickness (the being preset as 2.8 microns) requirement of film layer, determine entire Sedimentation time 60 minutes, entire sedimentation time is then divided into 1/3/6, wherein the sedimentation time of TiAl transition zone is entire deposition The sedimentation time of 10%, the TiAlN middle layer of the time of process is the 30% of the time of entire deposition process, outermost layer The sedimentation time of TiCrAlN film layer is the 60% of the time of entire deposition process.
9, the indoor ar pressure of plated film the determination of the preparation process of TiAl transition zone: is maintained at 2.2 × 10-1Pa, 2 The arc current of titanium-aluminum alloy target is placed in 58 amperes, and hard alloy substrate back bias voltage is -220 volts, and arcing time is entire deposition The 10% of the time of process, that is, 6 minutes, then adjusting ar pressure was 0, and nitrogen pressure reaches 2.8 × 10-1Pa is ready for The deposition of the TiAlN middle layer of the superhard composite coating of TiAl/TiAlN/TiZrAlN.
10, the indoor nitrogen pressure of plated film the determination of the preparation process of TiAlN middle layer: is maintained at 2.8 × 10-1Pa, 2 The arc current of a titanium-aluminum alloy target is placed in 56 amperes, and hard alloy substrate back bias voltage is -200 volts, and arcing time is entire heavy The 30% of the time of product process, i.e., 18 minutes.Then adjustment nitrogen pressure is 2.6 × 10-1Pa is ready for TiAl/TiAlN/ The deposition of the outermost layer TiZrAlN film layer of the superhard composite coating of TiZrAlN.
11, the determination of the preparation process of outermost layer TiZrAlN film layer: the indoor nitrogen pressure of plated film is maintained at 2.6 × 10-1The arc current of pa, 2 titanium-aluminum alloy targets and 2 titanium-zirconium alloy targets is placed in 60 amperes, and hard alloy substrate back bias voltage is- 180 volts, arcing time is the 60% of the time of entire deposition process, that is, 36 minutes.
12, the control of plated film room temperature: refer to obtain the plating of TiAl/TiAlN/TiZrAlN superhard composite film layer and determination The limitation of film room temperature, after hard alloy substrate completes entire coating process, plated film room temperature is 335 degrees Celsius;
13, work rest rotates: in coating chamber slow heating baking, carrying out ion bombardment, plating to hard alloy substrate It is always maintained at work rest rotation during the entire process of TiAl transition zone, TiAlN middle layer and outermost layer TiZrAlN film layer, turns Speed is 6 revs/min.
The superhard composite coating of TiAl/TiAlN/TiCrAlN for using the above method to prepare is measured, coating layer thickness It is 2.75 microns, using microhardness testers, under 25g power load, the hardness for measuring the superhard composite coating reaches 4400HV.
It will be understood by those skilled in the art that above embodiments are only exemplary embodiments, without departing substantially from spirit herein In the case where range, a variety of variations can be carried out, replaced and changed.

Claims (10)

1. a kind of method for preparing TiAl/TiAlN/TiZrAlN composite coating, comprising:
Select the titanium-aluminum alloy target that two Ti/Al atomic ratios are 50/50 and the titanium-zirconium alloy that two Ti/Zr atomic ratios are 45/55 Target;
Metallic matrix to be coated is placed on the work rest of coating chamber;
Pre-firing processes are carried out to the coating chamber;
Pre- Bombardment and cleaning technique is carried out to metallic matrix;
TiAl layers are plated on the metallic matrix, arcing time is at the first time;
TiAlN layers are plated on the TiAl layer, arcing time was the second time;
TiZrAlN layers are plated on the TiAlN layer, arcing time is the third time;
Wherein, the ratio of the first time, second time and the third time are 1:3:6.
2. according to the method described in claim 1, wherein, the titanium-aluminum alloy target that two Ti/Al atomic ratios are 50/50 is in the plating In 90 degree of configurations in film room, the titanium-zirconium alloy target that two Ti/Zr atomic ratios are 45/55 is in the coating chamber in 90 degree of configurations.
3. according to the method described in claim 1, wherein, the metallic matrix is high-speed steel or hard alloy, and is being incited somebody to action Before metallic matrix to be coated is placed on the work rest of coating chamber, decontamination, polishing, ultrasonic cleaning are carried out to the metallic matrix And drying process.
4. according to the method described in claim 1, wherein, the film surface to be plated and titanium-aluminum alloy target and titanium zirconium of the metallic matrix The distance on the surface of alloys target is in 25-30cm.
5. according to the method described in claim 1, wherein, carrying out pre-firing processes to the coating chamber includes: in the plated film The vacuum degree of room reaches 3 × 10-2When pa, starting baking electric current, the temperature of the coating chamber reach 200 DEG C used in the time it is not low In 20 minutes.
6. according to the method described in claim 1, wherein, carrying out pre- Bombardment and cleaning technique to metallic matrix includes: when the plating The back end vacuum degree of film room reaches 8.0 × 10-3Pa, prebake conditions temperature are filled with argon gas when reaching 200 DEG C, make the pressure of the coating chamber Reach 2.2 × 10 by force-1Pa~2.8 × 10-1Pa, opens each alloys target arc source, keep arc current stablize 55~60 amperes it Between, it carries out ion bombardment 15 minutes, bombards bias from 350 volts and progressively increase to 400 volts.
7. according to the method described in claim 1, wherein, plating TiAl layers on the metallic matrix includes: by the coating chamber Interior ar pressure is maintained at 2.2 × 10-1Pa~2.8 × 10-1The arc current of pa, two titanium-aluminum alloy targets is placed in 55~60 Between ampere, the back bias voltage of the metallic matrix is set as -220 volts, and the first time is no more than 10 minutes.
8. according to the method described in claim 1, wherein, it includes: to adjust ar pressure to be that TiAlN layers are plated on the TiAl layer 0, so that nitrogen pressure is reached 2.6 × 10-1Pa~2.8 × 10-1Pa, the arc current of two titanium-aluminum alloy targets are placed in 55~60 peaces Between training, the back bias voltage of the metallic matrix is set as -200 volts.
9. according to the method described in claim 1, wherein, plating TiZrAlN layers on the TiAlN layer includes: by the plated film Indoor nitrogen pressure is maintained at 2.8 × 10-1The arc current of pa, two titanium-aluminum alloy targets and two titanium-zirconium alloy targets is placed in Between 60-62 amperes, the back bias voltage of the metallic matrix is set as -180 volts.
10. the TiAl/TiAlN/TiZrAlN composite coating of method preparation according to any one of claim 1 to 9.
CN201810875578.XA 2018-08-03 2018-08-03 TiAl/TiAlN/TiZrAlN composite coating and preparation method thereof Pending CN108950488A (en)

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