CN104726835A - Preparation method for niobium nitride/ titanium aluminum nitride zirconium-niobium quaternary double-layered nitride film - Google Patents
Preparation method for niobium nitride/ titanium aluminum nitride zirconium-niobium quaternary double-layered nitride film Download PDFInfo
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- CN104726835A CN104726835A CN201510173560.1A CN201510173560A CN104726835A CN 104726835 A CN104726835 A CN 104726835A CN 201510173560 A CN201510173560 A CN 201510173560A CN 104726835 A CN104726835 A CN 104726835A
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Abstract
A preparation method for a niobium nitride/ titanium aluminum nitride zirconium-niobium quaternary double-layered nitride film comprises the following steps of (1) determinng a deposition technology; (2) using a target composition; (3) selecting and pre-treating workpieces; (4) performing pre-bombarding technology; (5) performing a deposition technology; (6) performing a heating and cooling-down technology; and (7) rotating the workpieces. By the preparation method for the niobium nitride/ titanium aluminum nitride zirconium-niobium quaternary double-layered nitride film, high hardness and high film/base binding force of the film are guaranteed, the wear resistance of the film is improved, and the high-temperature-resistant oxidation performance of the film is greatly improved. Moreover, the preparation method is simple and is easy to operate, the work efficiency is greatly improved, and the film plating cost is reduced.
Description
Technical field
The present invention relates to the preparation method of a kind of niobium nitride/TiAlN zirconium niobium quaternary dual layer nitride film.
Background technology
Multi-arc ion coating has that ionization level is high, depositing temperature is low, rate of film build is fast, bonding force is strong, Thin Film Tissue is fine and close and processing parameter is easy to the advantages such as adjustment.This technology is applicable to the preparation of composite ganoine film, and the application that succeeds in the preparation of titanium Quito unit individual layer, multi-element double-layer and the polynary gradient hard films such as titanium nitride, TiAlN, TiAlN zirconium and TiAlN zirconium chromium.
For the nitride film of titanium aluminium zirconium niobium four constituent element, it has the hardness higher than quaternary nitride films such as the ternary nitride films such as the binary nitride films such as unitary nitride film, the TiAlNs such as titanium nitride, TiAlN zirconium, TiAlN niobium and TiAlN zirconium chromium, better wear resistance and more excellent high temperature oxidation resistance, so TiAlN zirconium niobium quaternary nitride hard film has more excellent development prospect.
For the TiAlN zirconium niobium system quaternary film of single layer structure, there is some difference for the thermal expansivity of itself and matrix and Young's modulus, and the matching on stuctures and properties is also general.So the main drawback of this film is its hardness, film/base bonding force, wear resisting property and high temperature oxidation resistance can not meet cutting requirement under extremely mal-condition.
For the TiAlN zirconium niobium system quaternary film of gradient-structure, although the hardness of film, film/base bonding force, wear resisting property and high temperature oxidation resistance improves greatly, but the main drawback of this film is its preparation method relative complex, usual needs regulate nitrogen flow or target arc current always continuously, and efficiency is lower.
So in view of over-all properties and the preparation cost of cutter film, niobium nitride/TiAlN zirconium niobium quaternary dual layer nitride film is under the pressure of exploitation.
Summary of the invention
The object of the present invention is to provide the preparation method of a kind of niobium nitride/TiAlN zirconium niobium quaternary dual layer nitride film.This preparation method not only ensure that high rigidity and the high film/base bonding force of film, improves the wear resisting property of film, especially greatly improves the high temperature oxidation resistance of film; And the method is simple to operation, substantially increase working efficiency, reduce coating cost.
To achieve these goals, the present invention takes following technical scheme: a kind of niobium nitride/TiAlN zirconium niobium quaternary dual layer nitride film, four described constituent elements are titanium, aluminium, zirconium and niobium element, and bilayer structure take niobium nitride as transition layer, with TiAlN zirconium niobium for top layer.
A preparation method for niobium nitride/TiAlN zirconium niobium quaternary dual layer nitride film, comprises successively:
1. the determination of deposition technique: determine that multi sphere ion plating technology is the deposition technique of niobium nitride/TiAlN zirconium niobium hard films.
2. the selecting of target material composition: select the array mode of a niobium target and three Mallory sharton alloy targets as arc source, four targets are mutually 90 degree of configurations, and niobium target purity is 99.99%, titanium in Mallory sharton alloy target: aluminium: atomic percent zirconium is 65:30:5.
3. the selection of workpiece and pretreatment technology: workpiece selects Wimet and rapid steel actual cut cutter, its surface uses metal detergent to carry out, and routine is deoiled, decontamination process, then polished finish is carried out, finally use acetone and ethanol to carry out ultrasonic cleaning respectively, load vacuum chamber after drying and prepare plated film.
4. bombard technique in advance: before cvd nitride niobium/TiAlN zirconium niobium quaternary dual layer nitride film, carry out ion bombardment technique in advance, when coating chamber back end vacuum tightness reaches 10
-3handkerchief, temperature pass into reactant gases nitrogen when reaching 260 ~ 270 degrees Celsius, when coating chamber vacuum tightness reaches 2.5 ' 10
-1~ 3.0 ' 10
-1during handkerchief, open four arc sources simultaneously and carry out ion bombardment 15 minutes, the arc current of Mallory sharton alloy target controls to be 80 amperes, and the arc current of niobium target controls to be 60 amperes, and bombardment bias voltage control is 350 volts.
5. depositing operation: the concrete technology of cvd nitride niobium/TiAlN zirconium niobium quaternary dual layer nitride film, be divided into two stages, first stage cvd nitride niobium transition layer, remains on 2.5 ' 10 by the nitrogen pressure in coating chamber
-1~ 3.0 ' 10
-1handkerchief, close the arc current of Mallory sharton alloy target, the arc current of niobium target is still placed in 60 amperes, and it is 100 ~ 200 volts that workpiece bias controls, and depositing time is 40 minutes; Subordinate phase depositing titanium nitride aluminium zirconium niobium top layer, still remains on 2.5 ' 10 by the nitrogen pressure in coating chamber
-1~ 3.0 ' 10
-1handkerchief, reopens the arc current of Mallory sharton alloy target, is placed in 80 amperes, and the arc current of niobium target is still placed in 60 amperes, and it is 100 ~ 200 volts that workpiece bias controls, and depositing time is 20 minutes.
6. heat process for cooling: workpiece carries out electric heating element Baking out before bombarding technique in advance, and heat-up rate controls, in 3 ~ 5 degrees celsius/minute, to reach 260 ~ 270 degrees Celsius after 1 hour; Deposition process terminates also to carry out heated baking to the double-deck hard films of deposited niobium nitride/TiAlN zirconium niobium afterwards, small area analysis is adopted to carry out micro-heating 10 ~ 15 minutes, the arc current of Mallory sharton alloy target and niobium target is down to 20 amperes gradually from 80 amperes and 60 amperes respectively, close the arc current of all targets subsequently, workpiece cools to room temperature with the furnace.
7. workpiece rotating technics: in the whole process of film preparation, holding workpiece rotates always, and during cvd nitride niobium transition layer, transmission shaft voltage is 45 volts, and during depositing titanium nitride aluminium zirconium niobium top layer, transmission shaft voltage is 35 volts, and it is 4 ~ 10 revs/min that rotating speed controls.Niobium nitride/TiAlN zirconium niobium quaternary dual layer nitride film can be obtained according to the method described above.
Advantage of the present invention and application:
Compared with the existing technology, the present invention adopts bilayer structure due to film, makes preparation technology simple to operation, avoids the cumbersome approaches such as continuous adjusting process parameter when preparing Gradient Film, improves working efficiency, for production line operation provides possibility; Adding due to niobium nitride transition layer simultaneously, make this invention achieve high rigidity (>=HV4000) and the high film/base bonding force (> 200N) of film simultaneously, improve the wear resisting property (frictional coefficient ≈ 0.25 ~ 0.4) of film, especially greatly improve the high temperature oxidation resistance (oxidation resistance temperature ≈ 800oC) of film, its performance index are suitable with TiAlN zirconium niobium system Gradient Film.This niobium nitride/TiAlN zirconium niobium quaternary dual layer nitride film is mainly used in the surface of cutting tool and mould.
Embodiment
Embodiment 1
WC-8%Co inserted drill is prepared niobium nitride/TiAlN zirconium niobium quaternary dual layer nitride film, and its method is:
1. the determination of deposition technique: determine that multi sphere ion plating technology is the deposition technique of niobium nitride/TiAlN zirconium niobium quaternary dual layer nitride film.
2. the selecting of target material composition: select the array mode of a niobium target and three Mallory sharton alloy targets as arc source, four targets are mutually 90 degree of configurations, and niobium target purity is 99.99%, titanium in Mallory sharton alloy target: aluminium: atomic percent zirconium is 65:30:5.
3. the selection of workpiece and pretreatment technology: WC-8%Co inserted drill selected by workpiece, its surface uses metal detergent to carry out, and routine is deoiled, decontamination process, then carry out polished finish, finally use acetone and ethanol to carry out ultrasonic cleaning respectively, load vacuum chamber after drying and prepare plated film.
4. bombard technique in advance: before cvd nitride niobium/TiAlN zirconium niobium quaternary dual layer nitride film, carry out ion bombardment technique in advance, when coating chamber back end vacuum tightness reaches 10
-3handkerchief, temperature pass into reactant gases nitrogen when reaching 260 degrees Celsius, when coating chamber vacuum tightness reaches 2.5 ' 10
-1during handkerchief, open four arc sources simultaneously and carry out ion bombardment 15 minutes, the arc current of Mallory sharton alloy target controls to be 80 amperes, and the arc current of niobium target controls to be 60 amperes, and bombardment bias voltage control is 350 volts.
5. depositing operation: utilize multi sphere ion plating technology to prepare niobium nitride/TiAlN zirconium niobium quaternary dual layer nitride film in WC-8%Co hard alloy workpiece, concrete coated film deposition technological process is divided into two stages, first stage cvd nitride niobium transition layer, remains on 2.5 ' 10 by the nitrogen pressure in coating chamber
-1handkerchief, close the arc current of Mallory sharton alloy target, the arc current of niobium target is still placed in 60 amperes, and it is 200 volts that workpiece bias controls, and depositing time is 40 minutes; Subordinate phase depositing titanium nitride aluminium zirconium niobium top layer, still remains on 2.5 ' 10 by the nitrogen pressure in coating chamber
-1handkerchief, reopens the arc current of Mallory sharton alloy target, is placed in 80 amperes, and the arc current of niobium target is still placed in 60 amperes, and it is 200 volts that workpiece bias controls, and depositing time is 20 minutes.
6. heat process for cooling: workpiece carries out electric heating element Baking out before bombarding technique in advance, and heat-up rate controls, in 3 ~ 5 degrees celsius/minute, to reach 260 degrees Celsius after 1 hour; Deposition process terminates also to carry out heated baking to deposited niobium nitride/TiAlN zirconium niobium hard films afterwards, small area analysis is adopted to carry out micro-heating 15 minutes, the arc current of Mallory sharton alloy target and niobium target is down to 20 amperes gradually from 80 amperes and 60 amperes respectively, close the arc current of all targets subsequently, workpiece cools to room temperature with the furnace.
7. workpiece rotating technics: in the whole process of film preparation, holding workpiece rotates always, and during cvd nitride niobium transition layer, transmission shaft voltage is 45 volts, and during depositing titanium nitride aluminium zirconium niobium top layer, transmission shaft voltage is 35 volts, and it is 4 ~ 10 revs/min that rotating speed controls.
8. pair double-deck hard films of the niobium nitride/TiAlN zirconium niobium using aforesaid method to prepare on WC-8%Co inserted drill carries out performance test, film/base the bonding force of this quaternary dual layer nitride film is up to more than 200N, hardness is up to HV4200, frictional coefficient is low to moderate 0.25 ~ 0.35, and oxidation resistance temperature is up to 800oC.
Embodiment 2
W18Cr4V rapid steel milling cutter is prepared niobium nitride/TiAlN zirconium niobium quaternary dual layer nitride film, and its method is:
1. the determination of deposition technique: determine that multi sphere ion plating technology is the deposition technique of niobium nitride/TiAlN zirconium niobium quaternary dual layer nitride film.
2. the selecting of target material composition: select the array mode of a niobium target and three Mallory sharton alloy targets as arc source, four targets are mutually 90 degree of configurations, and niobium target purity is 99.99%, titanium in Mallory sharton alloy target: aluminium: atomic percent zirconium is 65:30:5.
3. the selection of workpiece and pretreatment technology: W18Cr4V rapid steel milling cutter selected by workpiece, its surface uses metal detergent to carry out, and routine is deoiled, decontamination process, then carry out polished finish, finally use acetone and ethanol to carry out ultrasonic cleaning respectively, load vacuum chamber after drying and prepare plated film.
4. bombard technique in advance: before cvd nitride niobium/TiAlN zirconium niobium quaternary dual layer nitride film, carry out ion bombardment technique in advance, when coating chamber back end vacuum tightness reaches 10
-3handkerchief, temperature pass into reactant gases nitrogen when reaching 260 degrees Celsius, when coating chamber vacuum tightness reaches 2.5 ' 10
-1handkerchief, open four arc sources simultaneously and carry out ion bombardment 15 minutes, the arc current of Mallory sharton alloy target remains on 80 amperes, and the arc current of niobium target remains on 60 amperes, and bombardment bias voltage is 350 volts.
5. depositing operation: utilize multi sphere ion plating technology to prepare niobium nitride/TiAlN zirconium niobium quaternary dual layer nitride film in WC-8%Co hard alloy workpiece, concrete depositing operation is divided into two stages, first stage cvd nitride niobium transition layer, remains on 2.5 ' 10 by the nitrogen pressure in coating chamber
-1handkerchief, close the arc current of Mallory sharton alloy target, the arc current of niobium target is still placed in 60 amperes, and it is 150 volts that workpiece bias controls, and depositing time is 40 minutes; Subordinate phase depositing titanium nitride aluminium zirconium niobium top layer, still remains on 2.5 ' 10 by the nitrogen pressure in coating chamber
-1handkerchief, reopens the arc current of Mallory sharton alloy target, is placed in 80 amperes, and the arc current of niobium target is still placed in 60 amperes, and it is 150 volts that workpiece bias controls, and depositing time is 20 minutes.
6. heat process for cooling: workpiece carries out electric heating element Baking out before bombarding technique in advance, and heat-up rate controls, in 3 ~ 5 degrees celsius/minute, to reach 260 degrees Celsius after 1 hour; Deposition process terminates also to carry out heated baking to deposited niobium nitride/TiAlN zirconium niobium hard films afterwards, small area analysis is adopted to carry out micro-heating 15 minutes, the arc current of Mallory sharton alloy target and niobium target is down to 20 amperes gradually from 80 amperes and 60 amperes respectively, close the arc current of all targets subsequently, workpiece cools to room temperature with the furnace.
7. workpiece rotating technics: in the whole process of film preparation, holding workpiece rotates always, and during cvd nitride niobium transition layer, transmission shaft voltage is 45 volts, and during depositing titanium nitride aluminium zirconium niobium top layer, transmission shaft voltage is 35 volts, and it is 4 ~ 10 revs/min that rotating speed controls.
8. pair double-deck hard films of the niobium nitride/TiAlN zirconium niobium using aforesaid method to prepare on W18Cr4V rapid steel milling cutter carries out performance test, film/base the bonding force of this quaternary dual layer nitride film is up to more than 200N, hardness is up to HV4000, frictional coefficient is low to moderate 0.3 ~ 0.4, and oxidation resistance temperature is up to 850oC.
Claims (1)
1. the preparation method of niobium nitride/TiAlN zirconium niobium quaternary dual layer nitride film, it is characterized in that: four described constituent elements are titanium, aluminium, zirconium and niobium element, bilayer structure take niobium nitride as transition layer, with TiAlN zirconium niobium for top layer, the preparation method of a kind of niobium nitride/TiAlN zirconium niobium quaternary dual layer nitride film comprises successively: the determination of (1), deposition technique: determine that multi sphere ion plating technology is the deposition technique of niobium nitride/TiAlN zirconium niobium hard films; (2), the selecting of target material composition: select the array mode of a niobium target and three Mallory sharton alloy targets as arc source, four targets are mutually 90 degree of configurations, and niobium target purity is 99.99%, titanium in Mallory sharton alloy target: aluminium: atomic percent zirconium is 65:30:5; (3), the selection of workpiece and pretreatment technology: workpiece selects Wimet and rapid steel actual cut cutter, its surface uses metal detergent to carry out, and routine is deoiled, decontamination process, then polished finish is carried out, finally use acetone and ethanol to carry out ultrasonic cleaning respectively, load vacuum chamber after drying and prepare plated film; (4), in advance technique is bombarded: before cvd nitride niobium/TiAlN zirconium niobium quaternary dual layer nitride film, carry out ion bombardment technique in advance, when coating chamber back end vacuum tightness reaches 10
-3handkerchief, temperature pass into reactant gases nitrogen when reaching 260 ~ 270 degrees Celsius, when coating chamber vacuum tightness reaches 2.5 ' 10
-1~ 3.0 ' 10
-1during handkerchief, open four arc sources simultaneously and carry out ion bombardment 15 minutes, the arc current of Mallory sharton alloy target controls to be 80 amperes, and the arc current of niobium target controls to be 60 amperes, and bombardment bias voltage control is 350 volts; (5), depositing operation: the concrete technology of cvd nitride niobium/TiAlN zirconium niobium quaternary dual layer nitride film, be divided into two stages, first stage cvd nitride niobium transition layer, remains on 2.5 ' 10 by the nitrogen pressure in coating chamber
-1~ 3.0 ' 10
-1handkerchief, close the arc current of Mallory sharton alloy target, the arc current of niobium target is still placed in 60 amperes, and it is 100 ~ 200 volts that workpiece bias controls, and depositing time is 40 minutes; Subordinate phase depositing titanium nitride aluminium zirconium niobium top layer, still remains on 2.5 ' 10 by the nitrogen pressure in coating chamber
-1~ 3.0 ' 10
-1handkerchief, reopens the arc current of Mallory sharton alloy target, is placed in 80 amperes, and the arc current of niobium target is still placed in 60 amperes, and it is 100 ~ 200 volts that workpiece bias controls, and depositing time is 20 minutes; (6), process for cooling is heated: workpiece carries out electric heating element Baking out before bombarding technique in advance, and heat-up rate controls, in 3 ~ 5 degrees celsius/minute, to reach 260 ~ 270 degrees Celsius after 1 hour; Deposition process terminates also to carry out heated baking to the double-deck hard films of deposited niobium nitride/TiAlN zirconium niobium afterwards, small area analysis is adopted to carry out micro-heating 10 ~ 15 minutes, the arc current of Mallory sharton alloy target and niobium target is down to 20 amperes gradually from 80 amperes and 60 amperes respectively, close the arc current of all targets subsequently, workpiece cools to room temperature with the furnace; (7), workpiece rotating technics: in the whole process of film preparation, holding workpiece rotates always, during cvd nitride niobium transition layer, transmission shaft voltage is 45 volts, during depositing titanium nitride aluminium zirconium niobium top layer, transmission shaft voltage is 35 volts, and it is 4 ~ 10 revs/min that rotating speed controls; Niobium nitride/TiAlN zirconium niobium quaternary dual layer nitride film can be obtained according to the method described above.
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110438442A (en) * | 2019-07-23 | 2019-11-12 | 江西科技师范大学 | A kind of nano silicon nitride niobium aluminium yttrium/amorphous silicon nitride two-phase superhard coating and its deposition method |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110438442A (en) * | 2019-07-23 | 2019-11-12 | 江西科技师范大学 | A kind of nano silicon nitride niobium aluminium yttrium/amorphous silicon nitride two-phase superhard coating and its deposition method |
| CN110438442B (en) * | 2019-07-23 | 2021-07-23 | 江西科技师范大学 | Nano niobium aluminum yttrium nitride/amorphous silicon nitride biphase superhard coating and deposition method thereof |
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