CN103484822A - Preparation method of titanium nitride aluminum zirconium/titanium nitride aluminum zirconium chromium multi-element double-layer hard film - Google Patents
Preparation method of titanium nitride aluminum zirconium/titanium nitride aluminum zirconium chromium multi-element double-layer hard film Download PDFInfo
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Abstract
The invention relates to a preparation method of a titanium nitride aluminum zirconium/titanium nitride aluminum zirconium chromium multi-element double-layer hard film. The preparation method comprises the steps: 1, determination of a deposition technology; 2, selection of target material components; 3, a workpiece selecting and preprocessing process; 4, a pre-bombarding process; 5, a deposition process; 6, a heating and cooling process; 7, a workpiece rotating process; 8, the titanium nitride aluminum zirconium/titanium nitride aluminum zirconium chromium multi-element double-layer hard film can be obtained according to the preparation method provided by the invention. According to the preparation method of the titanium nitride aluminum zirconium/titanium nitride aluminum zirconium chromium multi-element double-layer hard film, the binding force between the film and a matrix is enhanced, the heat resistance of the film is enhanced, in particular, the hardness and the wear resistance of the film are improved; the method is simple and easy to operate, the work efficiency is greatly improved, and the cost of film coating is reduced.
Description
Technical field
The present invention relates to a kind of preparation method of polynary double-deck hard reaction film, particularly relate to the preparation method of a kind of TiAlN zirconium/polynary double-deck hard films of TiAlN zirconium chromium.
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, film dense structure and processing parameter are easy to the advantages such as adjusting.This technology is applicable to the preparation of multicomponent composite ganoine film, and in the application that succeeds aspect the preparation of the titanium Quito such as titanium nitride, TiAlN, TiAlN zirconium and TiAlN chromium unit's individual layer and polynary gradient hard film.
TiAlN zirconium chromium quaternary nitride hard film has the hardness higher than ternary nitride hard films such as the binary nitride hard film such as monobasic nitride hard film, the TiAlNs such as titanium nitride and TiAlN zirconium, TiAlN chromium, better wear resistance and more excellent resistance toheat, so TiAlN zirconium chromium quaternary nitride hard film has good development prospect.
TiAlN zirconium chromium for single layer structure is the quaternary film, and there is some difference for the thermal expansivity of itself and matrix and Young's modulus, and the matching on structure and performance is also general.So the main drawback of this film is that its hardness, film/base bonding force, wear resisting property and resistance toheat can not meet the cutting requirement under mal-condition extremely.
TiAlN zirconium chromium for gradient-structure is the quaternary film, although the hardness of film, film/base bonding force, wear resisting property and resistance toheat are improved greatly, but the main drawback of this film is its preparation method relative complex, usually need to regulate continuously nitrogen flow or target arc current, efficiency is lower always.
Summary of the invention
The object of the present invention is to provide the preparation method of a kind of TiAlN zirconium/polynary double-deck hard films of TiAlN zirconium chromium, this preparation method has not only strengthened bonding force and the resistance toheat between film and matrix, has especially improved hardness and the wear resisting property of film; And the method is simple to operation, greatly improved working efficiency, reduced coating cost.
To achieve these goals, the present invention takes following technical scheme: a kind of TiAlN zirconium/polynary double-deck hard films of TiAlN zirconium chromium, and described bilayer structure is to take the TiAlN zirconium as transition layer, the TiAlN zirconium chromium of take is top layer.
The preparation method of a kind of TiAlN zirconium/polynary double-deck hard films of TiAlN zirconium chromium comprises successively:
1. deposition technique is definite: determine the deposition technique that multi sphere ion plating technology is the double-deck hard reaction film of TiAlN zirconium/TiAlN zirconium chromium.
2. selecting of target composition: select the array mode of a chromium target and two Mallory sharton alloy targets, three targets are mutually 90 degree configurations, and middle arc source is the chromium target, and purity is 99.99%, and arc source, both sides is the Mallory sharton alloy target, titanium: aluminium: atomic percent zirconium is 63:32:5.
3. the selection of workpiece and pretreatment technology: the selection Wimet is workpiece material, workpiece surface is used metal detergent to carry out that routine is deoiled, decontamination is processed, then carry out polished finish, finally use respectively acetone and ethanol to carry out ultrasonic cleaning, the vacuum chamber of packing into after oven dry is prepared plated film.
4. bombard in advance technique: before the double-deck hard reaction film of depositing titanium nitride aluminium zirconium/TiAlN zirconium chromium, carry out in advance ion bombardment technique, when coating chamber back end vacuum tightness reaches 10
-3handkerchief, temperature pass into reactant gases nitrogen while reaching 240 ~ 260 degrees centigrade, when coating chamber vacuum tightness reaches 2.5 ' 10
-1~ 3.0 ' 10
-1during handkerchief, open three arc sources simultaneously and carry out ion bombardment 10 minutes, it is 70 amperes that the arc current of Mallory sharton alloy target is controlled, and it is 40 amperes that the arc current of chromium target is controlled, and the bombardment bias voltage control is 350 volts.
5. depositing operation: the concrete technology of the double-deck hard reaction film of depositing titanium nitride aluminium zirconium/TiAlN zirconium chromium, be divided into two stages, first stage depositing titanium nitride aluminium zirconium transition layer, remain on 2.5 ' 10 by the nitrogen pressure in coating chamber
-1~ 3.0 ' 10
-1handkerchief, close the arc current of chromium target, and the arc current of Mallory sharton alloy target still is placed in 70 amperes, and it is 150 ~ 200 volts that workpiece bias is controlled, and depositing time is 30 minutes; Subordinate phase depositing titanium nitride aluminium zirconium chromium top layer, still remain on 2.5 ' 10 by the nitrogen pressure in coating chamber
-1~ 3.0 ' 10
-1handkerchief, reopen the arc current of chromium target, is placed in 40 amperes, and the arc current of Mallory sharton alloy target still is placed in 70 amperes, and it is 150 ~ 200 volts that workpiece bias is controlled, and depositing time is 20 minutes.
6. heating process for cooling: workpiece carries out the electric heating element Baking out before bombarding in advance technique, and heat-up rate is controlled at 3 ~ 5 degrees celsius/minute, reaches 240 ~ 260 degrees centigrade after 1 hour; After deposition process finishes, the double-deck hard reaction film of deposited TiAlN zirconium/TiAlN zirconium chromium is carried out to the post-heating baking, adopt little electric current to carry out micro-heating 10 ~ 15 minutes, the arc current of Mallory sharton alloy target and chromium target is down to 20 amperes gradually from 70 amperes and 40 amperes respectively, close subsequently the arc current of all targets, workpiece cools to room temperature with the furnace and gets final product.
7. workpiece rotating technics: in the whole process of film preparation, holding workpiece rotation always, transmission shaft voltage is 35 volts, it is 6 ~ 12 rev/mins that rotating speed is controlled.
8. according to preparation method of the present invention, can obtain above-mentioned TiAlN zirconium/polynary double-deck hard films of TiAlN zirconium chromium, this duplicature has the premium propertiess such as film/base bonding force strong (>200N), hardness large (>=HV3900), frictional coefficient low (≈ 0.25 ~ 0.35) and resistance to high temperature oxidation temperature high (≈ 700oC).
Compared with the existing technology, the present invention, because film adopts bilayer structure, makes preparation technology simple to operation, and while having avoided preparing Gradient Film, the cumbersome approaches such as continuous adjusting process parameter, improved working efficiency, for production line operation provides may; While, because TiAlN zirconium transition layer adds, makes this invention improve bonding force and the resistance toheat between film and matrix, has especially improved hardness and the wear resisting property of film, and its performance index and TiAlN zirconium chromium are that Gradient Film is suitable.The polynary double-deck hard films of this TiAlN zirconium/TiAlN zirconium chromium is mainly used in the surface of cutting tool, mould.
Embodiment
Embodiment
Embodiment 1
Prepare the polynary double-deck hard reaction film of TiAlN zirconium/TiAlN zirconium chromium on WC-8%Co Wimet workpiece, its method is:
1. deposition technique is definite: determine the deposition technique that multi sphere ion plating technology is the double-deck hard reaction film of TiAlN zirconium/TiAlN zirconium chromium.
2. selecting of target composition: select the array mode of a chromium target and two Mallory sharton alloy targets, three targets are mutually 90 degree configurations, and middle arc source is the chromium target, and purity is 99.99%, and arc source, both sides is the Mallory sharton alloy target, titanium: aluminium: atomic percent zirconium is 63:32:5.
3. the selection of workpiece and pretreatment technology: select the WC-8%Co Wimet as workpiece material, workpiece surface is used metal detergent to carry out that routine is deoiled, decontamination is processed, then carry out polished finish, finally use respectively acetone and ethanol to carry out ultrasonic cleaning, the vacuum chamber of packing into after oven dry is prepared plated film.
4. bombard in advance technique: before the double-deck hard reaction film of depositing titanium nitride aluminium zirconium/TiAlN zirconium chromium, carry out in advance ion bombardment technique, when coating chamber back end vacuum tightness reaches 10
-3handkerchief, temperature pass into reactant gases nitrogen while reaching 240 degrees centigrade, when coating chamber vacuum tightness reaches 2.5 ' 10
-1during handkerchief, open three arc sources simultaneously and carry out ion bombardment 10 minutes, it is 70 amperes that the arc current of Mallory sharton alloy target is controlled, and it is 40 amperes that the arc current of chromium target is controlled, and the bombardment bias voltage control is 350 volts.
5. depositing operation: utilize multi sphere ion plating technology to prepare the double-deck hard reaction film of TiAlN zirconium/TiAlN zirconium chromium on WC-8%Co Wimet workpiece, concrete coated film deposition technological process is divided into two stages, first stage depositing titanium nitride aluminium zirconium transition layer, remain on 2.5 ' 10 by the nitrogen pressure in coating chamber
-1handkerchief, close the arc current of chromium target, and the arc current of Mallory sharton alloy target still is placed in 70 amperes, and it is 150 volts that workpiece bias is controlled, and depositing time is 30 minutes; Subordinate phase depositing titanium nitride aluminium zirconium chromium top layer, still remain on 2.5 ' 10 by the nitrogen pressure in coating chamber
-1handkerchief, reopen the arc current of chromium target, is placed in 40 amperes, and the arc current of Mallory sharton alloy target still is placed in 70 amperes, and it is 150 volts that workpiece bias is controlled, and depositing time is 20 minutes.
6. heating process for cooling: workpiece carries out the electric heating element Baking out before bombarding in advance technique, and heat-up rate is controlled at 3 ~ 5 degrees celsius/minute, reaches 240 degrees centigrade after 1 hour; After deposition process finishes, the double-deck hard reaction film of deposited TiAlN zirconium/TiAlN zirconium chromium is carried out to the post-heating baking, adopt little electric current to carry out micro-heating 15 minutes, the arc current of Mallory sharton alloy target and chromium target is down to 20 amperes gradually from 70 amperes and 40 amperes respectively, close subsequently the arc current of all targets, workpiece cools to room temperature with the furnace and gets final product.
7. workpiece rotating technics: in the whole process of film preparation, holding workpiece rotation always, transmission shaft voltage is 35 volts, it is 6 ~ 12 rev/mins that rotating speed is controlled.
8. the double-deck hard reaction film of the TiAlN zirconium prepared on the WC-8%Co Wimet by the use aforesaid method/TiAlN zirconium chromium carries out performance test, the film of this bilayer hard reaction film/base bonding force is up to more than 200N, hardness is up to HV3900, frictional coefficient is low to moderate 0.3 ~ 0.35, and the resistance to high temperature oxidation temperature is up to 700oC.
Embodiment 2
Prepare the polynary double-deck hard reaction film of TiAlN zirconium/TiAlN zirconium chromium on WC-8%Co Wimet workpiece, its method is:
1. deposition technique is definite: determine the deposition technique that multi sphere ion plating technology is the double-deck hard reaction film of TiAlN zirconium/TiAlN zirconium chromium.
2. selecting of target composition: select the array mode of a chromium target and two Mallory sharton alloy targets, three targets are mutually 90 degree configurations, and middle arc source is the chromium target, and purity is 99.99%, and arc source, both sides is the Mallory sharton alloy target, titanium: aluminium: atomic percent zirconium is 63:32:5.
3. the selection of workpiece and pretreatment technology: select the WC-8%Co Wimet as workpiece material, workpiece surface is used metal detergent to carry out that routine is deoiled, decontamination is processed, then carry out polished finish, finally use respectively acetone and ethanol to carry out ultrasonic cleaning, the vacuum chamber of packing into after oven dry is prepared plated film.
4. bombard in advance technique: before the double-deck hard reaction film of depositing titanium nitride aluminium zirconium/TiAlN zirconium chromium, carry out in advance ion bombardment technique, when coating chamber back end vacuum tightness reaches 10
-3handkerchief, temperature pass into reactant gases nitrogen while reaching 260 degrees centigrade, when coating chamber vacuum tightness reaches 2.5 ' 10
-1handkerchief, open three arc sources simultaneously and carry out ion bombardment 10 minutes, and the arc current of Mallory sharton alloy target remains on 70 amperes, and the arc current of chromium target remains on 40 amperes, and the bombardment bias voltage is 350 volts.
5. depositing operation: utilize multi sphere ion plating technology to prepare the double-deck hard reaction film of TiAlN zirconium/TiAlN zirconium chromium on WC-8%Co Wimet workpiece, concrete depositing operation is divided into two stages, first stage depositing titanium nitride aluminium zirconium transition layer, remain on 2.5 ' 10 by the nitrogen pressure in coating chamber
-1handkerchief, close the arc current of chromium target, and the arc current of Mallory sharton alloy target still is placed in 70 amperes, and it is 200 volts that workpiece bias is controlled, and depositing time is 30 minutes; Subordinate phase depositing titanium nitride aluminium zirconium chromium top layer, still remain on 2.5 ' 10 by the nitrogen pressure in coating chamber
-1handkerchief, reopen the arc current of chromium target, is placed in 40 amperes, and the arc current of Mallory sharton alloy target still is placed in 70 amperes, and it is 200 volts that workpiece bias is controlled, and depositing time is 20 minutes.
6. heating process for cooling: workpiece carries out the electric heating element Baking out before bombarding in advance technique, and heat-up rate is controlled at 3 ~ 5 degrees celsius/minute, reaches 260 degrees centigrade after 1 hour; After deposition process finishes, the double-deck hard reaction film of deposited TiAlN zirconium/TiAlN zirconium chromium is carried out to the post-heating baking, adopt little electric current to carry out micro-heating 15 minutes, the arc current of Mallory sharton alloy target and chromium target is down to 20 amperes gradually from 70 amperes and 40 amperes respectively, close subsequently the arc current of all targets, workpiece cools to room temperature with the furnace and gets final product.
7. workpiece rotating technics: in the whole process of film preparation, holding workpiece rotation always, transmission shaft voltage is 35 volts, it is 6 ~ 12 rev/mins that rotating speed is controlled.
8. the double-deck hard reaction film of the TiAlN zirconium prepared on the WC-8%Co Wimet by the use aforesaid method/TiAlN zirconium chromium carries out performance test, the film of this bilayer hard reaction film/base bonding force is up to more than 200N, hardness is up to HV4000, frictional coefficient is low to moderate 0.25 ~ 0.35, and the resistance to high temperature oxidation temperature is up to 700oC.
Claims (1)
1. the preparation method of TiAlN zirconium/polynary double-deck hard films of TiAlN zirconium chromium, it is characterized in that: described bilayer structure is to take the TiAlN zirconium as transition layer, the TiAlN zirconium chromium of take is top layer, and the preparation method of a kind of TiAlN zirconium/polynary double-deck hard films of TiAlN zirconium chromium comprises successively: the determining of (1), deposition technique: determine the deposition technique that multi sphere ion plating technology is the double-deck hard reaction film of TiAlN zirconium/TiAlN zirconium chromium; (2), selecting of target composition: the array mode of selecting a chromium target and two Mallory sharton alloy targets, three targets are mutually 90 degree configurations, and middle arc source is the chromium target, and purity is 99.99%, arc source, both sides is the Mallory sharton alloy target, titanium: aluminium: atomic percent zirconium is 63:32:5; (3), the selection of workpiece and pretreatment technology: the selection Wimet is workpiece material, workpiece surface is used metal detergent to carry out that routine is deoiled, decontamination is processed, then carry out polished finish, finally use respectively acetone and ethanol to carry out ultrasonic cleaning, the vacuum chamber of packing into after oven dry is prepared plated film; (4) bombard, in advance technique: before the double-deck hard reaction film of depositing titanium nitride aluminium zirconium/TiAlN zirconium chromium, carry out in advance ion bombardment technique, when coating chamber back end vacuum tightness reaches 10
-3handkerchief, temperature pass into reactant gases nitrogen while reaching 240 ~ 260 degrees centigrade, when coating chamber vacuum tightness reaches 2.5 ' 10
-1~ 3.0 ' 10
-1during handkerchief, open three arc sources simultaneously and carry out ion bombardment 10 minutes, it is 70 amperes that the arc current of Mallory sharton alloy target is controlled, and it is 40 amperes that the arc current of chromium target is controlled, and the bombardment bias voltage control is 350 volts; (5), depositing operation: the concrete technology of the double-deck hard reaction film of depositing titanium nitride aluminium zirconium/TiAlN zirconium chromium, be divided into two stages, first stage depositing titanium nitride aluminium zirconium transition layer, remain on 2.5 ' 10 by the nitrogen pressure in coating chamber
-1~ 3.0 ' 10
-1handkerchief, close the arc current of chromium target, and the arc current of Mallory sharton alloy target still is placed in 70 amperes, and it is 150 ~ 200 volts that workpiece bias is controlled, and depositing time is 30 minutes; Subordinate phase depositing titanium nitride aluminium zirconium chromium top layer, still remain on 2.5 ' 10 by the nitrogen pressure in coating chamber
-1~ 3.0 ' 10
-1handkerchief, reopen the arc current of chromium target, is placed in 40 amperes, and the arc current of Mallory sharton alloy target still is placed in 70 amperes, and it is 150 ~ 200 volts that workpiece bias is controlled, and depositing time is 20 minutes; (6), heating process for cooling: workpiece carries out the electric heating element Baking out before bombarding in advance technique, and heat-up rate is controlled at 3 ~ 5 degrees celsius/minute, reaches 240 ~ 260 degrees centigrade after 1 hour; After deposition process finishes, the double-deck hard reaction film of deposited TiAlN zirconium/TiAlN zirconium chromium is carried out to the post-heating baking, adopt little electric current to carry out micro-heating 10 ~ 15 minutes, the arc current of Mallory sharton alloy target and chromium target is down to 20 amperes gradually from 70 amperes and 40 amperes respectively, close subsequently the arc current of all targets, workpiece cools to room temperature with the furnace and gets final product; (7), workpiece rotating technics: in the whole process of film preparation, holding workpiece is rotated always, and transmission shaft voltage is 35 volts, and it is 6 ~ 12 rev/mins that rotating speed is controlled; (8), according to preparation method of the present invention, can obtain above-mentioned TiAlN zirconium/polynary double-deck hard films of TiAlN zirconium chromium, this duplicature has the premium propertiess such as film/base bonding force strong (>200N), hardness large (>=HV3900), frictional coefficient low (≈ 0.25 ~ 0.35) and resistance to high temperature oxidation temperature high (≈ 700oC).
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104726824A (en) * | 2015-04-14 | 2015-06-24 | 沈阳大学 | Titanium nitride-aluminium-zirconium/titanium nitride-aluminium-zirconium-silicon quaternary double layer nitride film preparation method |
| CN106319449A (en) * | 2016-10-25 | 2017-01-11 | 郑州航空工业管理学院 | Anti-erosion gradient film for compressor blades of aviation turbojet engine and preparation method of anti-erosion gradient film |
| CN108950488A (en) * | 2018-08-03 | 2018-12-07 | 河北工程大学 | TiAl/TiAlN/TiZrAlN composite coating and preparation method thereof |
| CN109097743A (en) * | 2018-09-16 | 2018-12-28 | 烟台大学 | A kind of superhard W-Cr-Al-Ti-N nanometer gradient multilayer film and preparation method thereof |
| RU2808481C1 (en) * | 2023-04-14 | 2023-11-28 | Федеральное государственное унитарное предприятие "Всероссийский научно-исследовательский институт авиационных материалов" Национального исследовательского центра "Курчатовский институт" (НИЦ "Курчатовский институт" - ВИАМ) | Method for producing erosion-corrosion-resistant coating on surface of titanium alloy product |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104726824A (en) * | 2015-04-14 | 2015-06-24 | 沈阳大学 | Titanium nitride-aluminium-zirconium/titanium nitride-aluminium-zirconium-silicon quaternary double layer nitride film preparation method |
| CN106319449A (en) * | 2016-10-25 | 2017-01-11 | 郑州航空工业管理学院 | Anti-erosion gradient film for compressor blades of aviation turbojet engine and preparation method of anti-erosion gradient film |
| CN108950488A (en) * | 2018-08-03 | 2018-12-07 | 河北工程大学 | TiAl/TiAlN/TiZrAlN composite coating and preparation method thereof |
| CN109097743A (en) * | 2018-09-16 | 2018-12-28 | 烟台大学 | A kind of superhard W-Cr-Al-Ti-N nanometer gradient multilayer film and preparation method thereof |
| RU2808481C1 (en) * | 2023-04-14 | 2023-11-28 | Федеральное государственное унитарное предприятие "Всероссийский научно-исследовательский институт авиационных материалов" Национального исследовательского центра "Курчатовский институт" (НИЦ "Курчатовский институт" - ВИАМ) | Method for producing erosion-corrosion-resistant coating on surface of titanium alloy product |
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Application publication date: 20140101 |