CN106282936A - A kind of preparation method of chromium nitride coating - Google Patents
A kind of preparation method of chromium nitride coating Download PDFInfo
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- CN106282936A CN106282936A CN201510275833.3A CN201510275833A CN106282936A CN 106282936 A CN106282936 A CN 106282936A CN 201510275833 A CN201510275833 A CN 201510275833A CN 106282936 A CN106282936 A CN 106282936A
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Abstract
The invention belongs to metal material surface deposition hard coat field, be specifically related to the preparation method of a kind of chromium nitride (CrN) coating.The method is by during arc ion plating, an axial magnetic-field coil is applied outside negative electrode Cr target, its axial magnetic field produced is made to carry out arc speckle retraining control, accelerate spots moving speed, purpose in matrix surface depositing high-quality CrN coating, it is thus achieved that there is higher hardness and high tenacity and there is the CrN coating of relatively low-friction coefficient.The present invention is suitable for various cutter, mould and metallic element surface deposition CrN coating, to improve performance and the usage life-span of this workpiece further.
Description
Technical field:
The invention belongs to metal material surface deposition hard coat field, be specifically related to a kind of chromium nitride (CrN)
The preparation method of coating.
Background technology:
At present, along with the development of country's advanced manufacturing technology, traditional hard alloy or high-speed steel tool are carried
Go out the highest requirement.Machining technique with Digit Control Machine Tool as representative just towards at a high speed, in high precision, high
The directions such as reliability are developed.NC cutting tool surface-coating technology, especially with CVD and PVD prepare with
TiN is that the coated cutting tool of representative obtains a wide range of applications during the working (machining) efficiency improving various alloys, with
And be subsequently developed that were the coatings such as TiC, TiCN, TiAlN, AlTiN, CrAlN and be developed and obtain reality
Application.But the high temperature being because in working angles to the oxidation of coating, chip to the adhesive wear of coating and painting
The brittleness problems of layer itself, a processing difficult problem for above-mentioned alloy is not solved.Such as, TiAlN coating
There is high rigidity and good high temperature oxidation resistance, hence it is evident that improve working (machining) efficiency and cutter life, but
Its higher fragility and coefficient of friction, limit the coatings such as TiAlN at high speed, dry cutting and difficult cutting alloy etc.
The application of material, also limit its actual application in terms of high-precision mold and other wear resistant friction reducing workpiece coating.
Compared with in above coating, CrN coating is preferably combined with alloy substrate owing to having relatively low coefficient of friction
The features such as power, higher toughness and corrosion resistance, are widely used in a large amount of wear-resisting structure such as automobile piston rings, mould
On part.But due to the lower hardness of CrN coating, generally HV1600～HV2000, it is unfavorable for its wearability
Raising, then seem when demand higher to hardness unable to do what one wishes.
How on the basis of not increasing coefficient of friction, to improve hardness further, become what current CrN coating faced
Matter of utmost importance.Although developed multi-element coating such as CrAlN and laminated coating such as Cr/CrN later, but due to cost
Increase or process complexity, economically consider to still suffer from some problems.
Therefore, prepare a kind of CrN coating that can have higher hardness and high tenacity and there is relatively low-friction coefficient,
The most necessary to raising tool and mould performance and service life further.
Summary of the invention
For the deficiency of existing coating material system, it is an object of the invention to provide and a kind of there is higher hardness
The preparation method of CrN coating, it is thus achieved that there is higher hardness and high tenacity and there is the CrN painting of relatively low-friction coefficient
Layer.
The technical scheme is that
The preparation method of a kind of chromium nitride coating, during arc ion plating, applies outside negative electrode Cr target
One axial magnetic-field coil so that it is arc speckle is carried out retraining control by the axial magnetic field of generation, accelerates spots moving speed
Degree, in matrix surface depositing high-quality CrN coating.
The preparation method of described chromium nitride coating, utilizes arc ion plating apparatus to deposit coating, its detailed process
For: workpiece cleaning to be plated is put into after drying in the vacuum chamber of electric arc ion-plating deposition device, be evacuated to vacuum
House vacuum degree reaches 1 × 10-3Pa～6 × 10-3During Pa, open negative electrode Cr arc simultaneously, arc stream control 60～
200A, workpiece is biased as-500～-1000V；Sample is proceeded ion bom bardment 1～5 minutes；After
Adjusting substrate bias is-100～-600V scopes, is passed through argon, and air pressure is 0.1～1.0Pa, deposits Cr transition
Layer 1～10 minute；Rear regulation pack field coil electric current is 0.5～5A, and magnetic induction scope is 10～200
Gauss, is passed through nitrogen, and adjusting air pressure is 0.5～5.0Pa, and substrate bias is-200～-600V；The plated film time is
30～120 minutes；After deposition terminates, close rapidly cathode arc on and off switch；Close substrate bias；Stop gas
Body is passed through, and continues to be evacuated to workpiece and cools to less than 80 DEG C with the furnace, and coating process terminates, and opens vacuum chamber,
Take out workpiece.
The preparation method of described chromium nitride coating, gained CrN nano-composite coating outward appearance is silver gray, scanning
The gross thickness of Electronic Speculum testing coating is 1～5 micron, and nano-indenter test coating hardness is 20～25GPa, and sound is sent out
Penetrating scratching instrument testing coating adhesion is 40～80N, and coefficient of friction is 0.35～0.5.
Compared with prior art, advantages of the present invention and providing the benefit that:
1, the present invention is at the coating that surface of the work forms the transition zone that formed by Cr film and CrN layer is constituted, film
Base junction makes a concerted effort to reach more than 70N, and coating hardness reaches more than HV2000.
2, compared with traditional arc ion plating preparation method, due to the fact that and be arranged around axial magnetic at target
Field coil is to produce axial magnetic field, and this magnetic field can make spots moving speed accelerate, not only increase target from
Rate, and in coating process, luminous intensity substantially increases, and illustrates to also promote the ionization of nitrogen, and this is the most quite
In defining ion beam assisted depositing, promote the densification of coating.
Accompanying drawing illustrates:
Fig. 1 is electric arc ion plating device schematic diagram of the present invention.Wherein, magnetic field is made up of 1 solenoid,
Magnetic induction can be regulated by coil current.
In figure: 1 vacuum chamber；2 work stage；3 workpiece；4 targets；5 solenoids；6 solenoid support
Cylinder；7 solenoid power supplys；8 pulsed bias power supplies；9 work stage rotating shafts.
Detailed description of the invention:
As it is shown in figure 1, electric arc ion plating device of the present invention specifically includes that vacuum chamber 1, work stage 2, workpiece
3, target 4, solenoid 5, solenoid support cylinder 6, solenoid power supply 7, pulsed bias power supply 8,
Work stage rotating shaft 9 etc., concrete structure is as follows:
Arranging workpiece 3 in work stage 2 in vacuum chamber 1, electromagnetic wire is passed through in target 4 (negative electrode Cr target) outside
Circle support cylinder 6 arranges axial magnetic coil 5, and solenoid power supply 7 is connected with solenoid 5.Pulse is inclined
The positive pole of voltage source 8 is connected with vacuum chamber 1 outer wall, bottom the negative pole of pulsed bias power supply 8 and work stage 2
Work stage rotating shaft 9 connects.
In a specific embodiment, the present invention, by during arc ion plating, executes outside negative electrode Cr target
Add an axial magnetic-field coil so that it is arc speckle is carried out retraining control by the axial magnetic field of generation, accelerates spots moving
Speed, in the purpose of matrix surface depositing high-quality CrN coating, specifically comprises the following steps that
(1) plating transition zone: use High Pure Chromium target, when vacuum house vacuum degree reaches 1 × 10-3Pa～6 × 10-3Pa
Time, vacuum chamber is heated to 300～500 DEG C；Opening negative electrode Cr arc, arc stream controls 60～200A simultaneously,
Workpiece is biased as-500～-1000V, and workpiece proceeds ion bom bardment 1～5 minutes；Rear adjustment matrix
Bias is-100～-600V scopes, is passed through argon, and air pressure is 0.1～1.0Pa, deposits Cr transition zone 1～10
Minute.
(2) plating CrN layer: stop argon, logical nitrogen, nitrogen flow controls 10～200sccm, sets gas
Pressure is 0.5～5Pa scope；Matrix is applied pulsed negative bias-200V～-600V；Regulation Cr target current be 70～
150A, regulation axial magnetic-field coil electric current is 0.5～5A simultaneously, and magnetic induction scope is 10～200 Gausses,
Sedimentation time is 30～120 minutes；
(3) deposition terminate after, stop rapidly arc, stop matrix pulsed negative bias, stop be passed through gas, continue to take out
Vacuum, workpiece cools to less than 80 DEG C with the furnace, and whole coating procedures terminates.
Below by embodiment, the present invention is further elaborated on.
Embodiment 1
Plating transition zone: base material uses high-speed steel (trade mark is W18Cr4V), and specimen size is
20mm × 10mm × 10mm, coated surface a size of 20mm × 10mm.Plated film front surface first pass through grinding,
Polishing, ultrasonic cleaning, dried, put on vacuum chamber sample stage, in treating vacuum chamber, vacuum reaches 4 × 10-3Pa
Time, vacuum chamber is heated to 400 DEG C, matrix adds pulsed negative bias-800V, opens chromium target arc source, arc stream simultaneously
Stable at 70A, sample is carried out Cr ion bom bardment 5 minutes；Adjust pulsed negative bias to-300V, be passed through argon,
Air pressure is 0.5Pa, deposition Cr film 3 minutes；Hereafter, enter plating CrN layer deposition process, first stop argon and lead to
Entering nitrogen, adjustment air pressure is 0.5Pa；Adjusting matrix pulsed negative bias is-400V, and adjustment target current is 80A,
Regulation pack field coil electric current is 0.5A simultaneously, and magnetic induction scope is 20 Gausses, and sedimentation time is 60
Minute；After deposition terminates, stop rapidly arc, stop matrix pulsed negative bias, stop being passed through gas, continue evacuation,
Workpiece cools to less than 80 DEG C with the furnace, and galvanization process terminates.
Gained CrN nano-composite coating outward appearance is silver gray, and the gross thickness of sem test coating is 3.1 micro-
Rice；Nano-indenter test coating hardness is 21.6GPa, and acoustic emission scratching instrument testing coating adhesion is 72N,
Coefficient of friction is 0.42.
Embodiment 2
Base material uses 304 rustless steels, and specimen size is 20mm × 10mm × 10mm, and coated surface is a size of
20mm×10mm.Plated film front surface first passes through grinding, polishing, ultrasonic cleaning, dried, puts into vacuum chamber
On sample stage, in treating vacuum chamber, vacuum reaches 3 × 10-3During Pa, vacuum chamber being heated to 420 DEG C, matrix adds
Pulsed negative bias-700V, opens chromium target arc source simultaneously, and arc stream is stable at 70A, sample carries out Cr ion and bangs
Hit 2 minutes；Adjusting pulsed negative bias to-300V, be passed through argon, air pressure is 0.3Pa, deposition Cr film 2 minutes；
Hereafter, entering plating CrN layer deposition process, first stop argon and be passed through nitrogen, adjustment air pressure is 1.0Pa；Adjust
Matrix pulsed negative bias is-300V, and adjustment target current is 90A, and regulation pack field coil electric current is simultaneously
1.0A, magnetic induction scope is 60 Gausses, and sedimentation time is 40 minutes；Deposition terminate after, stop rapidly arc,
Stopping matrix pulsed negative bias, stop being passed through gas, continue evacuation, workpiece cools to less than 80 DEG C with the furnace, plating
Layer process terminates.
Gained CrN nano-composite coating outward appearance is silver gray, and the gross thickness of sem test coating is 2.0 micro-
Rice；Nano-indenter test coating hardness is 22.9GPa, and acoustic emission scratching instrument testing coating adhesion is 67N,
Coefficient of friction is 0.45.
Embodiment 3
Base material uses high-speed steel (trade mark is W6Mo5Cr4V2Al), and specimen size is
20mm × 10mm × 10mm, coated surface a size of 20mm × 10mm.Plated film front surface first passes through grinding, throws
Light, ultrasonic cleaning, dried, put on vacuum chamber sample stage, in treating vacuum chamber, vacuum reaches 3 × 10-3Pa
Time, vacuum chamber is heated to 400 DEG C, matrix adds pulsed negative bias-600V, opens chromium target arc source, arc stream simultaneously
Stable at 70A, sample is carried out Cr ion bom bardment 3 minutes；Adjust pulsed negative bias to-300V, be passed through argon,
Air pressure is 0.8Pa, deposition Cr film 4 minutes；Hereafter, enter plating CrN layer deposition process, first stop argon and lead to
Entering nitrogen, adjustment air pressure is 2.0Pa；Adjusting matrix pulsed negative bias is-300V, and adjustment target current is 90A,
Regulation pack field coil electric current is 2.0A simultaneously, and magnetic induction scope is 100 Gausses, and sedimentation time is 120
Minute；After deposition terminates, stop rapidly arc, stop matrix pulsed negative bias, stop being passed through gas, continue evacuation,
Workpiece cools to less than 80 DEG C with the furnace, and galvanization process terminates.
Gained CrN nano-composite coating outward appearance is silver gray, and the gross thickness of sem test coating is 6.2 micro-
Rice；Nano-indenter test coating hardness is 23.4GPa, and acoustic emission scratching instrument testing coating adhesion is 61N,
Coefficient of friction is 0.4.
Embodiment 4
Base material uses 316L rustless steel, and specimen size is 20mm × 10mm × 10mm, and coated surface is a size of
20mm×10mm.Plated film front surface first passes through grinding, polishing, ultrasonic cleaning, dried, puts into vacuum chamber
On sample stage, in treating vacuum chamber, vacuum reaches 4 × 10-3During Pa, vacuum chamber being heated to 440 DEG C, matrix adds
Pulsed negative bias-900V, opens chromium target arc source simultaneously, and arc stream is stable at 70A, sample carries out Cr ion and bangs
Hit 1 minute；Adjusting pulsed negative bias to-300V, be passed through argon, air pressure is 1.0Pa, deposition Cr film 5 minutes；
Hereafter, entering plating CrN layer deposition process, first stop argon and be passed through nitrogen, adjustment air pressure is 3.0Pa；Adjust
Matrix pulsed negative bias is-300V, and adjustment target current is 100A, and regulation pack field coil electric current is simultaneously
3.0A, magnetic induction scope is 150 Gausses, and sedimentation time is 60 minutes；Deposition terminate after, stop rapidly arc,
Stopping matrix pulsed negative bias, stop being passed through gas, continue evacuation, workpiece cools to less than 80 DEG C with the furnace, plating
Layer process terminates.
Gained CrN nano-composite coating outward appearance is silver gray, and the gross thickness of sem test coating is 3.5 micro-
Rice；Nano-indenter test coating hardness is 22.1GPa, and acoustic emission scratching instrument testing coating adhesion is 57N,
Coefficient of friction is 0.44.
Claims (3)
1. the preparation method of a chromium nitride coating, it is characterised in that: during arc ion plating, at the moon
An axial magnetic-field coil is applied so that it is arc speckle is carried out retraining control by the axial magnetic field of generation outside the Cr target of pole,
Accelerate spots moving speed, in matrix surface depositing high-quality CrN coating.
2. according to the preparation method of the chromium nitride coating described in claim 1, it is characterised in that utilize electric arc from
Sub-plating appts deposition coating, its detailed process is: workpiece cleaning to be plated is put into electric arc ion-plating deposition after drying
In the vacuum chamber of device, in being evacuated to vacuum chamber, vacuum reaches 1 × 10-3Pa～6 × 10-3During Pa, simultaneously
Opening negative electrode Cr arc, arc stream controls 60～200A, and workpiece is biased as-500～-1000V；To sample
Proceed ion bom bardment 1～5 minutes；Rear adjustment substrate bias is-100～-600V scopes, is passed through argon,
Air pressure is 0.1～1.0Pa, deposition Cr transition zone 1～10 minutes；Rear regulation pack field coil electric current be 0.5～
5A, magnetic induction scope is 10～200 Gausses, is passed through nitrogen, and adjusting air pressure is 0.5～5.0Pa, matrix
Bias is for-200～-600V；The plated film time is 30～120 minutes；After deposition terminates, close rapidly cathode arc electricity
Source switch；Close substrate bias；Stop gas being passed through, continue to be evacuated to workpiece and cool to less than 80 DEG C with the furnace,
Coating process terminates, and opens vacuum chamber, takes out workpiece.
3. according to the preparation method of the chromium nitride coating described in claim 1 or 2, it is characterised in that gained
CrN nano-composite coating outward appearance is silver gray, and the gross thickness of sem test coating is 1～5 micron, nanometer
Impression test coating hardness is 20～25GPa, and acoustic emission scratching instrument testing coating adhesion is 40～80N, rubs
Wiping coefficient is 0.35～0.5.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107227441A (en) * | 2017-05-11 | 2017-10-03 | 中国科学院力学研究所 | A kind of TiAlSiN coating productions based on reactive sputtering hesitation |
| CN108385073A (en) * | 2018-04-24 | 2018-08-10 | 信利（惠州）智能显示有限公司 | The production method of ito thin film |
| CN114150261A (en) * | 2021-11-30 | 2022-03-08 | 昆山英利悦电子有限公司 | Chromium nitride coating process for automobile sound panel |
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| CN102345101A (en) * | 2010-08-04 | 2012-02-08 | 中国科学院金属研究所 | Method for plating inner surface of long tube through arc ion plating with magnetic field and electric field enhancement |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107227441A (en) * | 2017-05-11 | 2017-10-03 | 中国科学院力学研究所 | A kind of TiAlSiN coating productions based on reactive sputtering hesitation |
| CN107227441B (en) * | 2017-05-11 | 2019-02-22 | 中国科学院力学研究所 | A kind of TiAlSiN coating production based on reactive sputtering hesitation |
| CN108385073A (en) * | 2018-04-24 | 2018-08-10 | 信利（惠州）智能显示有限公司 | The production method of ito thin film |
| CN114150261A (en) * | 2021-11-30 | 2022-03-08 | 昆山英利悦电子有限公司 | Chromium nitride coating process for automobile sound panel |
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Application publication date: 20170104 |