CN103805996A - Composite treating method for nitriding surface of metal material after coating - Google Patents
Composite treating method for nitriding surface of metal material after coating Download PDFInfo
- Publication number
- CN103805996A CN103805996A CN201410018736.1A CN201410018736A CN103805996A CN 103805996 A CN103805996 A CN 103805996A CN 201410018736 A CN201410018736 A CN 201410018736A CN 103805996 A CN103805996 A CN 103805996A
- Authority
- CN
- China
- Prior art keywords
- nitriding
- workpiece
- arc
- film
- ion
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
Abstract
The invention belongs to the field of material surface modification, and particularly relates to a composite treating method for nitriding the surface of a metal material after coating. The composite treating method is suitable for surface strengthening of tools, molds and metal accessories. The composite treating method comprises the following steps: firstly depositing a layer of nitride thin film on the surface of a metal material substrate by adopting magnetron sputtering or arc ion plating, wherein the thickness of the thin film is 0.1-50 micrometers; then carrying out ion nitriding treatment on the surface of the coating film by adopting an ion nitriding technology for 0.5-10 hours. Due to adoption of the composite treating method, the problem of low film-substrate bonding strength and the like caused by a black layer easily occurring in a composite treating process of coating after nitriding are solved. The workpiece obtained by adopting the coating-nitriding composite treating method of carrying out ion nitriding treatment after depositing a layer of thin film has the characteristics of high surface hardness, good wear resistance, high film-substrate binding force, reliable quality, stability and the like.
Description
Technical field:
The invention belongs to material surface modifying field, be specially the first plated film of a kind of metal material surface compounding method of nitriding again, be applicable to the surface strengthening of cutter, mould, metallic element.
Background technology:
Nitriding treatment, as a kind of hot chemical treatment process, generally can improve the antifatigue of steel, the wear-resistant resistance to corrosion that undermines.But the workpiece surface hardness after nitriding treatment is still lower, still can not meet the demand of growing harsh application conditions.
And the hard coats such as TiN prepared by employing physical gas-phase deposite method (Physical Vapour Deposition, PVD) have become most widely used top coat.Because TiN coating has the advantages such as high rigidity, high adhesion strength, low-friction coefficient and good chemical stability, be widely used in every field, especially tool industry.Along with the harshness day by day of application operating mode, TiN class hard coat can not meet the demand of tool and mould and some important workpiece surface.Major cause is that die steel matrix is softer, or the bonding force of coating and matrix is inadequate.Therefore the requirement that, relies on merely a certain treatment technology can not meet high-fatigue strength, high bending strength, high red hardness, low frictional wear and bear high-speed overload.
In order to solve the deficiency of single treatment technology, people [the A.S.Korhonen such as the scientist Korhnen of Finland, E.H.Sirvio, M.S.Sulonen.Plasma nitriding and ion plating with an intensified glow discharge.Thin Solid Films, 1983,107:387-394] propose pecvd nitride and physical gas-phase deposition to combine, and develop the new technology of a kind of pecvd nitride (Plasma Nitriding, PN)/physical vapor deposition (PVD) Combined Processing (PN/PVD).Why Combined Processing layer wearing quality improves, and is to have made its supporting capacity improve because nitrided case has improved the hardness of matrix, has both given hard and crisp coating with strong support, has reduced again the hardness gradient at film/base interface.Comparatively level and smooth hardness gradient, the stress while making to carry in coating reduces, the stress distribution of interface is more even, thereby brittle coating destroys or the possibility of cracking reduces, and wearing quality improves.
Because this composite treatment technology has the incomparable advantage of monotechnics, therefore since the nineties in 20th century, obtain broad research and concern, after its depositing device development, treatment process and workpiece are processed, structure and correlated performance etc. have carried out large quantity research.And, the material category of PN/PVD Combined Processing develops into even cast iron etc. of low alloy steel, stainless steel, die steel, aluminium and aluminium alloy, titanium or titanium alloy from initial carbon steel, along with the development of composite treatment technology, the material category of Combined Processing also can constantly expand.For example:
The Wang Li equality people [Wang Liping of the Lanzhou Chemistry and Physics Institute of the Chinese Academy of Sciences, Xue Qunji, Zhang Guangan. the preparation method of diamond-like composite coating on surface of piston ring. patent of invention: 200810150858.0] a kind of preparation method of diamond-like composite coating on surface of piston ring disclosed, the method is processed at piston ring surface and is formed one deck nitride layer by low-temperature plasma nitriding, and then adopt magnetic filtering cathode arc-magnetron sputtering composite deposition one deck non-hydrogen diamond film, to improve resistance to wearing and self-lubricating property of piston ring.
The people such as the Guo Qiuyan of Zhejiang Geely Automobile Research Institute Co., Ltd [Guo Qiuyan, Liu Guangyu, Li Li, Liu Qiang, Yang Anzhi, Zhao Fuquan. patent of invention: 201210194611.5] a kind of surface recombination processing method of steel die is disclosed, the method is first sprayed a watt processing to steel die after heat treatment, then form ion-nitriding layer by ionitriding at die surface, finally die surface is carried out to ion film plating again.The method steel die after treatment has improved its surface hardness, wear resistance and film substrate bond strength, has solved traditional moulds surface and has re-used the early stage technical problem of easily destroying.
The horse triumph of Xi'an Communications University, Xu Kewei [horse triumph, Xu Kewei. PCVO plasma impregnation composite reinforced method for precise vane hot forging die. patent of invention: 02114481.8] a kind of PCVO plasma impregnation composite reinforced method for precise vane hot forging die disclosed, the method is first put into industrial PCVD vacuum oven by the blade mold after quenching, tempering and is carried out plasma nitridation, rear employing PCVD depositing TiN or TiCN film.The mould of the method processing has improved surface hardness and film substrate bond strength, is applicable to harsher frictional wear condition.
Although nitriding-plated film Combined Processing has solved the deficiency of single nitriding, single coating process, Combined Processing layer has higher hardness, matrix supporting capacity and wear resistance, if but process application is improper, be easy to occur a black layer, the formation of black layer is due to the outer field nitride Fe of nitride layer in ion plating process
4n, Fe
2-3nitrogen in N is to external diffusion, thereby is transformed into ferrite.This ferrite lamellae not only hardness is very low, and has certain loosening, and can greatly reduce the film substrate bond strength of Combined Processing layer, has a strong impact on friction and wear behavior and the work-ing life of Combined Processing layer.
Summary of the invention:
In order to overcome the above problems, the object of the present invention is to provide the first plated film of a kind of metal material surface compounding method of nitriding again, adopt the metal works prepared of the method to have that surface hardness is high, film substrate bond strength is high, wear resistance is good and the advantage such as long service life, thereby promote better the performance of metal works.
Technical scheme of the present invention is:
The first plated film of a metal material surface compounding method for nitriding again, adopts vacuum coating method first to deposit one deck nitride film at metal material surface, after deposit film again through ionitriding processing.
The described first plated film of the metal material surface compounding method of nitriding again, vacuum coating method is magnetron sputtering or arc ions electroplating method.
The described first plated film of the metal material surface compounding method of nitriding again, nitride film is titanium nitride, chromium nitride, zirconium nitride, TiAlN, nitrogenize chrome-silicon, TiAlN silicon or chromium nitride aluminum film, film thickness is 0.1～50 micron.
The described first plated film of the metal material surface compounding method of nitriding again, ionitriding is treated to arc light ion nitriding and/or glow ion nitriding method.
The described first plated film of the metal material surface compounding method of nitriding again, when ionitriding is treated to arc light ion nitriding processing, is arranged on arc source in magnetron sputtering or arc ion plating apparatus.
The described first plated film of the metal material surface compounding method of nitriding again, comprises the steps:
(1) workpiece pre-treatment: pending workpiece, after oil removing, raw spirit ultrasonic cleaning, being dried, is placed in the sample table of magnetron sputtering or arc ion plating apparatus;
(2) vacuumize and workpiece preheating: start the pumped vacuum systems of magnetron sputtering or arc ion plating apparatus, treat that vacuum degree in vacuum chamber reaches 1 × 10
-2pa～5 × 10
-3when Pa, the workpiece in vacuum chamber is heated to 20～550 ℃ by heater;
(3) aura cleans: in vacuum chamber, pass into argon gas, air pressure is controlled between 0.5～2Pa, opens grid bias power supply, and bias voltage control, in-400V～-1000V scope, makes gas generation glow discharge, workpiece surface is carried out to aura and clean 5～60 minutes;
Adopt when arc ion plating (aip), after aura cleans, also need to open cathode arc target, carry out arc light ion Bombardment and cleaning, workpiece bias was controlled at-500～-1000V, to workpiece Bombardment and cleaning 1～10 minute;
(4) deposit film transition layer: pass into argon gas in vacuum chamber, air pressure is controlled between 0.1～2Pa, opens the target power supply in magnetron sputtering or arc ion plating simultaneously, and workpiece bias is controlled at-100～-600V, first deposit the transition layer of 100～500nm, depositing time is 1～30 minute;
(5) deposit film: pass into nitrogen in vacuum chamber, air pressure is controlled between 0.1～2Pa, workpiece bias is controlled at-50～-1500V, opens magnetic control or arc cathode target, depositing nitride film, the thin film deposition time is 20～300 minutes; After deposition finishes, close rapidly target power switch;
(6) nitriding processing: adopt arc light ion nitriding and/or glow ion nitriding technology to carry out ionitriding processing.
The first plated film of the described metal material surface compounding method of nitriding again, the workpiece surface after adopting arc light ion nitridation technique to deposit film carries out nitriding treatment process and is:
In the time that workpiece temperature is controlled at 300～650 ℃, modulation nitrogen pressure is between 0.1～1Pa, and workpiece bias is controlled at-400～-1500V, opens arc source heater supply, heated filament heating produces thermal electron emission, and the nitrogen molecule clashing in cathode tube makes it form nitrogen ion N
+; Then open arc discharge power supply, between cathode tube and vacuum-chamber wall, apply the direct supply of a 80～100V, thereby in cathode tube, produce arc discharge, form electric arc nitrogen plasma, under the focusing of focusing magnetic field and the effect of plasma electrically arc voltage, acceleration enters vacuum chamber, starts workpiece surface to carry out nitriding processing, and the treatment time is 30～300 minutes; After nitriding finishes, close rapidly arc source arc discharge power supply, heater supply and focusing magnetic field power supply, close workpiece bias power supply, stop gas and pass into, continue to vacuumize, workpiece cools to the furnace below 50 ℃, plated film-nitriding Combined Processing end of processing.
The first plated film of the described metal material surface compounding method of nitriding again, the workpiece surface after adopting glow ion nitriding technology to deposit film carries out nitriding treatment process and is:
Workpiece after deposit film, with packing in ion nitriding furnace after raw spirit ultrasonic cleaning, is evacuated to 5 × 10
-3pa～1 × 10
-2when Pa, the workpiece in nitriding furnace is heated to 400～550 ℃ by heater; In nitriding furnace, pass into ammonia, air pressure is controlled at 100～1000Pa, between anode nitriding furnace wall and cathode-workpiece, apply the direct supply of 400～800V, between anode and cathode, produce glow discharge and form nitrogen plasma, nitrogen ion accelerates to carry out nitriding processing to workpiece surface under the effect of workpiece bias electric field, and the treatment time is 0.5～40 hour; After nitriding finishes, close rapidly DC power supply switch, stop gas and pass into, continue to vacuumize, workpiece cools to the furnace below 50 ℃, and nitriding treating processes finishes.
Core concept of the present invention is:
Utilize magnetron sputtering or the arc ion plating (aip) Non-equilibrium in thin film deposition, the film of deposition has more defect and stoichiometric ratio can not reach desirable ratio completely, then carry out again ionitriding, nitrogen ion carries out thermodiffusion by these defective locations or other interstitial site etc. in film, through film base interface.And then, diffuse into 5～200 microns of workpiece surfaces, not only improve film substrate bond strength, and improved film hardness and wear resistance.
The invention has the beneficial effects as follows:
1, the present invention first adopts magnetron sputtering and/or arc ion plating to metal material surface, and first depositing a layer thickness at metal material surface is the nitride film of 0.1～50 micron, after again through the compounding method of arc light ion nitriding and/or glow ion nitriding.The prerequisite that film grain-size is little, defect concentration is high that the present invention utilizes magnetron sputtering or the arc ion plating (aip) non-equilibrium property in film deposition process to cause, after thin film deposition, film surface is carried out to ionitriding, can effectively reduce film defects density, improve film compactness.
2, the present invention carries out ionitriding after surface of workpiece ion film plating again, nitrogen ion has diffuseed to form the gradient of nitrogen at film and matrix workpiece surface, and be not easy to form the ferrite lamellae in " nitriding/plated film Combined Processing " process, effectively guaranteed the film substrate bond strength of Combined Processing layer.
3, the invention solves and in plated film Combined Processing process, be prone to the problems such as film substrate bond strength that black layer produces is low after first nitriding, compared with conventional nitriding/plated film composite treatment process, plated film/nitriding composite treatment process is more easily controlled, film substrate bond strength and film compactness are higher, can effectively improve surface of workpiece hardness, wear resistance and work-ing life.
Embodiment:
Below in conjunction with specific embodiment, the present invention is described in further detail.
Embodiment 1
(1) workpiece pre-treatment: workpiece adopts rapid steel (trade mark is W18Cr4V), and workpiece size is 20mm × 10mm × 10mm, and treat surface is of a size of 20mm × 10mm.Pending workpiece, after oil removing, raw spirit ultrasonic cleaning, being dried, is placed in the sample table of ionitriding/arc ion plating Combined Processing equipment;
(2) vacuumize and workpiece preheating: start the pumped vacuum systems of Combined Processing equipment, treat that vacuum degree in vacuum chamber reaches 5 × 10
-3when Pa, the workpiece in vacuum chamber is heated to 400 ℃ by heater;
(3) aura (or/and arc light) cleans: in vacuum chamber, pass into argon gas, air pressure is controlled at 2.0Pa, opens grid bias power supply, and bias voltage control, at-800V, makes gas generation glow discharge, workpiece surface is carried out to aura and clean 20 minutes; Then adjusting ar pressure is 0.8Pa, opens cathode arc pure titanium target, and target current is 80A, carries out arc light ion Bombardment and cleaning, and be controlled at-1000V of workpiece bias, to workpiece Bombardment and cleaning 5 minutes;
(4) deposit film transition layer: ar pressure maintains 0.8Pa, is adjusted into workpiece bias-600V, first deposits pure ti interlayer, and depositing time is 3 minutes, the thickness 150nm of pure ti interlayer;
(5) deposit film: pass into nitrogen in vacuum chamber, air pressure is controlled at 0.8Pa, be controlled at-500V of workpiece bias, the pure titanium target of cathode arc target current still maintains 80A, depositing TiN thin film, the thin film deposition time is 60 minutes; After deposition finishes, close rapidly target power switch;
(6) nitriding processing: in the time that workpiece temperature is controlled at 450 ℃, modulation nitrogen pressure is 0.6Pa, be controlled at-800V of workpiece bias, open focusing magnetic field power supply, electric current is set to 0.5A, opens arc source heater supply, and heater current is adjusted into 100A, heated filament heating produces thermal electron emission, and the nitrogen molecule clashing in cathode tube makes it form nitrogen ion N
+; Then open arc discharge power supply, between cathode tube and vacuum-chamber wall, apply the direct supply of a 80～100V, thereby in cathode tube, produce arc discharge, form electric arc nitrogen plasma, under the focusing of focusing magnetic field and the effect of plasma electrically arc voltage, acceleration enters vacuum chamber, starts workpiece surface to carry out nitriding processing, and the treatment time is 60 minutes; After nitriding finishes, close rapidly arc source arc discharge power supply, heater supply and focusing magnetic field power supply, close workpiece bias power supply, stop gas and pass into, continue to vacuumize, workpiece cools to the furnace below 50 ℃, plated film-nitriding Combined Processing end of processing.
After workpiece takes out, after sample preparation face is cut to after sticky, polishing with after the corrosion of 4wt% nital, testing its TiN film thickness is 3.2 microns, in rapid steel, nitriding depth is about 6 microns.Then, use respectively surface microhardness and the film substrate bond strength of microhardness tester and scratching instrument test compound processing layer, be respectively 26GPa and 75N.
Embodiment 2
(1) workpiece pre-treatment: workpiece adopts rapid steel (trade mark is W6Mo5Cr4V2Al), and workpiece size is 20mm × 10mm × 10mm, and treat surface is of a size of 20mm × 10mm.Pending workpiece, after oil removing, raw spirit ultrasonic cleaning, being dried, is placed in the sample table of ionitriding/arc ion plating Combined Processing equipment;
(2) vacuumize and workpiece preheating: start the pumped vacuum systems of Combined Processing equipment, treat that vacuum degree in vacuum chamber reaches 6 × 10
-3when Pa, the workpiece in vacuum chamber is heated to 430 ℃ by heater;
(3) aura (or/and arc light) cleans: in vacuum chamber, pass into argon gas, air pressure is controlled at 1.5Pa, opens grid bias power supply, and bias voltage control, at-750V, makes gas generation glow discharge, workpiece surface is carried out to aura and clean 20 minutes; Then adjusting ar pressure is 0.8Pa, opens cathode arc high purity titanium aluminium alloy (titanium aluminium part by weight is 7:3) target, and target current is 75A, carries out arc light ion Bombardment and cleaning, and be controlled at-1000V of workpiece bias, to workpiece Bombardment and cleaning 5 minutes;
(4) deposit film transition layer: ar pressure maintains 0.8Pa, is adjusted into workpiece bias-600V, first titanium deposition aluminium transition layer, and depositing time is 5 minutes, the thickness of titanium aluminium transition layer is 250nm;
(5) deposit film: pass into nitrogen in vacuum chamber, air pressure is controlled at 0.8Pa, be controlled at-500V of workpiece bias, cathode arc titanium aluminum alloy target current still maintains 80A, depositing Ti AlN film, the thin film deposition time is 60 minutes; After deposition finishes, close rapidly target power switch;
(6) nitriding processing: in the time that workpiece temperature is controlled at 450 ℃, modulation nitrogen pressure is 0.6Pa, be controlled at-800V of workpiece bias, open focusing magnetic field power supply, electric current is set to 0.5A, opens arc source heater supply, and heater current is adjusted into 100, heated filament heating produces thermal electron emission, and the nitrogen molecule clashing in cathode tube makes it form nitrogen ion N
+; Then open arc discharge power supply, between cathode tube and vacuum-chamber wall, apply the direct supply of a 80～100V, thereby in cathode tube, produce arc discharge, form electric arc nitrogen plasma, under the focusing of focusing magnetic field and the effect of plasma electrically arc voltage, acceleration enters vacuum chamber, starts workpiece surface to carry out nitriding processing, and the treatment time is 40 minutes; After nitriding finishes, close rapidly arc source arc discharge power supply, heater supply and focusing magnetic field power supply, close workpiece bias power supply, stop gas and pass into, continue to vacuumize, workpiece cools to the furnace below 50 ℃, plated film-nitriding Combined Processing end of processing.
After workpiece takes out, after sample preparation face is cut to after sticky, polishing with after the corrosion of 4wt% nital, testing its TiAlN film thickness is 3.6 microns, in rapid steel, nitriding depth is about 4 microns.Then, use respectively surface microhardness and the film substrate bond strength of microhardness tester and scratching instrument test compound processing layer, be respectively 32GPa and 72N.
Embodiment 3
(1) workpiece pre-treatment: workpiece adopts austenitic stainless steel (trade mark is 0Cr19Ni9), and workpiece size is Φ 30mm × 10mm, and treat surface is of a size of Φ 30mm × 10mm.Pending workpiece, after oil removing, raw spirit ultrasonic cleaning, being dried, is placed in the sample table of ionitriding/magnetron sputtering Combined Processing equipment;
(2) vacuumize and workpiece preheating: start the pumped vacuum systems of Combined Processing equipment, treat that vacuum degree in vacuum chamber reaches 5 × 10
-3when Pa, the workpiece in vacuum chamber is heated to 400 ℃ by heater;
(3) aura cleans: in vacuum chamber, pass into argon gas, air pressure is controlled at 2.0Pa, opens grid bias power supply, and bias voltage control, at-800V, makes gas generation glow discharge, workpiece surface is carried out to aura and clean 20 minutes;
(4) deposit film transition layer: ar pressure maintains 2.0Pa, is adjusted into workpiece bias-600V, first deposits pure ti interlayer, and depositing time is 3 minutes, and the thickness of pure ti interlayer is 180nm;
(5) deposit film: pass into nitrogen in vacuum chamber, air pressure is controlled at 0.8Pa, be controlled at-500V of workpiece bias, magnetic controlling target electric current still maintains 10A, depositing TiN thin film, the thin film deposition time is 120 minutes; After deposition finishes, close rapidly magnetic controlling target power switch;
(6) nitriding processing: in the time that workpiece temperature is controlled at 450 ℃, modulation nitrogen pressure is 0.6Pa, be controlled at-800V of workpiece bias, open focusing magnetic field power supply, electric current is set to 0.5A, opens arc source heater supply, and heater current is adjusted into 100A, heated filament heating produces thermal electron emission, and the nitrogen molecule clashing in cathode tube makes it form nitrogen ion N
+; Then open arc discharge power supply, between cathode tube and vacuum-chamber wall, apply the direct supply of a 80～100V, thereby in cathode tube, produce arc discharge, form electric arc nitrogen plasma, under the focusing of focusing magnetic field and the effect of plasma electrically arc voltage, acceleration enters vacuum chamber, starts workpiece surface to carry out nitriding processing, and the treatment time is 60 minutes; After nitriding finishes, close rapidly arc source arc discharge power supply, heater supply and focusing magnetic field power supply, close workpiece bias power supply, stop gas and pass into, continue to vacuumize, workpiece cools to the furnace below 50 ℃, plated film-nitriding Combined Processing end of processing.
After workpiece takes out, after sample preparation face is cut to after sticky, polishing with after the corrosion of 4wt% nital, testing its TiN film thickness is 2.2 microns, in stainless steel, nitriding depth is 2 microns.Then, use respectively surface microhardness and the film substrate bond strength of microhardness tester and scratching instrument test compound processing layer, be respectively 24GPa and 80N.
Embodiment 4
(1) workpiece pre-treatment: workpiece adopts rapid steel (trade mark is W18Cr4V), and workpiece size is 20mm × 10mm × 10mm, and treat surface is of a size of 20mm × 10mm.Pending workpiece, after oil removing, raw spirit ultrasonic cleaning, being dried, is placed in the sample table of arc ion plating apparatus;
(2) vacuumize and workpiece preheating: start the pumped vacuum systems of arc ion plating apparatus, treat that vacuum degree in vacuum chamber reaches 5 × 10
-3when Pa, the workpiece in vacuum chamber is heated to 400 ℃ by heater;
(3) aura (or/and arc light) cleans: in vacuum chamber, pass into argon gas, air pressure is controlled at 2.0Pa, opens grid bias power supply, and bias voltage control, at-800V, makes gas generation glow discharge, workpiece surface is carried out to aura and clean 20 minutes; Then adjusting ar pressure is 0.8Pa, opens cathode arc pure titanium target, and target current is 80A, carries out arc light ion Bombardment and cleaning, and be controlled at-1000V of workpiece bias, to workpiece Bombardment and cleaning 5 minutes;
(4) deposit film transition layer: ar pressure maintains 0.8Pa, is adjusted into workpiece bias-600V, first deposits pure ti interlayer, and depositing time is 3 minutes, and the thickness of pure ti interlayer is 150nm;
(5) deposit film: pass into nitrogen in vacuum chamber, air pressure is controlled at 0.8Pa, be controlled at-500V of workpiece bias, the pure titanium target of cathode arc target current still maintains 80A, depositing TiN thin film, the thin film deposition time is 60 minutes; After deposition finishes, close rapidly target power switch, close workpiece bias power supply, stop gas and pass into, continue to vacuumize, workpiece cools to 50 ℃ with the furnace and takes out sample when following;
(6) nitriding processing: after the workpiece ultrasonic cleaning after plated film, being dried, be placed in the sample table of glow ion nitriding furnace, be evacuated to 7 × 10
-3when Pa, heater, is heated to 550 ℃ by workpiece; Then in nitriding furnace, pass into ammonia, air pressure is 500Pa, between anode nitriding furnace wall and cathode-workpiece, apply the direct supply of 800V, between anode and cathode, produce glow discharge and form nitrogen plasma, between workpiece and nitriding furnace wall, produce glow discharge, start workpiece surface to carry out nitriding processing, the treatment time is 300 minutes; After nitriding finishes, close rapidly workpiece bias power supply, stop gas and pass into, continue to vacuumize, workpiece cools to the furnace below 50 ℃, and nitriding treating processes finishes.
After workpiece takes out, after sample preparation face is cut to after sticky, polishing with after the corrosion of 4wt% nital, testing its TiN film thickness is 3.1 microns, in rapid steel, nitriding depth is 10 microns.Then, use respectively surface microhardness and the film substrate bond strength of microhardness tester and scratching instrument test compound processing layer, be respectively 24GPa and 72N.
Embodiment result shows, first the present invention adopts magnetron sputtering or arc ions to be plated in metal material matrix surface deposition one deck nitride film, and film thickness is 0.1～50 micron; Then adopt ionitriding technology to carry out ionitriding processing to coated surface, the treatment time is 0.5～10 hour.The workpiece obtaining by the inventive method, has that surface hardness is high, wear resistance good, film-substrate cohesion is high, reliable in quality and a feature such as stable.
Claims (8)
1. the first plated film of a metal material surface compounding method for nitriding again, is characterized in that, adopts vacuum coating method first to deposit one deck nitride film at metal material surface, after deposit film again through ionitriding processing.
2. according to the first plated film of the metal material surface claimed in claim 1 compounding method of nitriding again, it is characterized in that, vacuum coating method is magnetron sputtering or arc ions electroplating method.
3. according to the first plated film of the metal material surface claimed in claim 1 compounding method of nitriding again, it is characterized in that, nitride film is titanium nitride, chromium nitride, zirconium nitride, TiAlN, nitrogenize chrome-silicon, TiAlN silicon or chromium nitride aluminum film, and film thickness is 0.1～50 micron.
4. according to the first plated film of the metal material surface claimed in claim 1 compounding method of nitriding again, it is characterized in that, ionitriding is treated to arc light ion nitriding and/or glow ion nitriding method.
5. according to the first plated film of the metal material surface claimed in claim 4 compounding method of nitriding again, it is characterized in that, when ionitriding is treated to arc light ion nitriding processing, arc source is arranged in magnetron sputtering or arc ion plating apparatus.
6. according to the first plated film of the metal material surface one of claim 1 to the 5 Suo Shu compounding method of nitriding again, it is characterized in that, comprise the steps:
(1) workpiece pre-treatment: pending workpiece, after oil removing, raw spirit ultrasonic cleaning, being dried, is placed in the sample table of magnetron sputtering or arc ion plating apparatus;
(2) vacuumize and workpiece preheating: start the pumped vacuum systems of magnetron sputtering or arc ion plating apparatus, treat that vacuum degree in vacuum chamber reaches 1 × 10
-2pa～5 × 10
-3when Pa, the workpiece in vacuum chamber is heated to 20～550 ℃ by heater;
(3) aura cleans: in vacuum chamber, pass into argon gas, air pressure is controlled between 0.5～2Pa, opens grid bias power supply, and bias voltage control, in-400V～-1000V scope, makes gas generation glow discharge, workpiece surface is carried out to aura and clean 5～60 minutes;
Adopt when arc ion plating (aip), after aura cleans, also need to open cathode arc target, carry out arc light ion Bombardment and cleaning, workpiece bias was controlled at-500～-1000V, to workpiece Bombardment and cleaning 1～10 minute;
(4) deposit film transition layer: pass into argon gas in vacuum chamber, air pressure is controlled between 0.1～2Pa, opens the target power supply in magnetron sputtering or arc ion plating simultaneously, and workpiece bias is controlled at-100～-600V, first deposit the transition layer of 100～500nm, depositing time is 1～30 minute;
(5) deposit film: pass into nitrogen in vacuum chamber, air pressure is controlled between 0.1～2Pa, workpiece bias is controlled at-50～-1500V, opens magnetic control or arc cathode target, depositing nitride film, the thin film deposition time is 20～300 minutes; After deposition finishes, close rapidly target power switch;
(6) nitriding processing: adopt arc light ion nitriding and/or glow ion nitriding technology to carry out ionitriding processing.
7. according to the first plated film of the metal material surface claimed in claim 6 compounding method of nitriding again, it is characterized in that, the workpiece surface after adopting arc light ion nitridation technique to deposit film carries out nitriding treatment process and is:
In the time that workpiece temperature is controlled at 300～650 ℃, modulation nitrogen pressure is between 0.1～1Pa, and workpiece bias is controlled at-400～-1500V, opens arc source heater supply, heated filament heating produces thermal electron emission, and the nitrogen molecule clashing in cathode tube makes it form nitrogen ion N
+; Then open arc discharge power supply, between cathode tube and vacuum-chamber wall, apply the direct supply of a 80～100V, thereby in cathode tube, produce arc discharge, form electric arc nitrogen plasma, under the focusing of focusing magnetic field and the effect of plasma electrically arc voltage, acceleration enters vacuum chamber, starts workpiece surface to carry out nitriding processing, and the treatment time is 30～300 minutes; After nitriding finishes, close rapidly arc source arc discharge power supply, heater supply and focusing magnetic field power supply, close workpiece bias power supply, stop gas and pass into, continue to vacuumize, workpiece cools to the furnace below 50 ℃, plated film-nitriding Combined Processing end of processing.
8. according to the first plated film of the metal material surface claimed in claim 7 compounding method of nitriding again, it is characterized in that, the workpiece surface after adopting glow ion nitriding technology to deposit film carries out nitriding treatment process and is:
Workpiece after deposit film, with packing in ion nitriding furnace after raw spirit ultrasonic cleaning, is evacuated to 5 × 10
-3pa～1 × 10
-2when Pa, the workpiece in nitriding furnace is heated to 400～550 ℃ by heater; In nitriding furnace, pass into ammonia, air pressure is controlled at 100～1000Pa, between anode nitriding furnace wall and cathode-workpiece, apply the direct supply of 400～800V, between anode and cathode, produce glow discharge and form nitrogen plasma, nitrogen ion accelerates to carry out nitriding processing to workpiece surface under the effect of workpiece bias electric field, and the treatment time is 0.5～40 hour; After nitriding finishes, close rapidly DC power supply switch, stop gas and pass into, continue to vacuumize, workpiece cools to the furnace below 50 ℃, and nitriding treating processes finishes.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410018736.1A CN103805996B (en) | 2014-01-16 | 2014-01-16 | The compounding method of the first plated film of a kind of metal material surface nitriding again |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410018736.1A CN103805996B (en) | 2014-01-16 | 2014-01-16 | The compounding method of the first plated film of a kind of metal material surface nitriding again |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN103805996A true CN103805996A (en) | 2014-05-21 |
| CN103805996B CN103805996B (en) | 2015-09-16 |
Family
ID=50703363
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201410018736.1A Active CN103805996B (en) | 2014-01-16 | 2014-01-16 | The compounding method of the first plated film of a kind of metal material surface nitriding again |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN103805996B (en) |
Cited By (25)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104561909A (en) * | 2015-01-27 | 2015-04-29 | 大连理工常州研究院有限公司 | Ionitriding/arc ion plating surface composite modification apparatus and method |
| CN104947143A (en) * | 2015-05-29 | 2015-09-30 | 华北水利水电大学 | Titanium-based TiNx/TiO2-RuO2 coating anode |
| CN105349941A (en) * | 2015-11-16 | 2016-02-24 | 哈尔滨工业大学 | Modification method for obtaining high-harness and high-wear-resistance gradient layer on surface of copper alloy |
| CN105568211A (en) * | 2015-12-29 | 2016-05-11 | 哈尔滨工业大学 | Method for enhancing diffusion of plasma on aluminum alloy surface |
| CN105908119A (en) * | 2016-04-23 | 2016-08-31 | 上海大学 | Surface oxidation treatment method of aluminum alloy extrusion die |
| RU2611003C1 (en) * | 2015-11-02 | 2017-02-17 | Федеральное государственное бюджетное образовательное учреждение высшего профессионального образования "Уфимский государственный авиационный технический университет" | Method of ion nitration of titanium alloys |
| RU2625518C2 (en) * | 2015-11-02 | 2017-07-14 | Федеральное государственное бюджетное образовательное учреждение высшего профессионального образования "Уфимский государственный авиационный технический университет" | Method of nitridation of titanic alloys in glow discharge |
| CN107937876A (en) * | 2017-12-29 | 2018-04-20 | 中国电子科技集团公司第四十三研究所 | A kind of TiAlN composite superhard coatings with the support of hardness gradient layer and preparation method thereof |
| CN108247191A (en) * | 2016-12-29 | 2018-07-06 | 核工业西南物理研究院 | A kind of method that hot isostatic pressing prevents welding assembly and jacket adhesion |
| CN108372281A (en) * | 2018-03-28 | 2018-08-07 | 北京鼎翰科技有限公司 | A kind of tubing casting method based on stainless steel and carbon steel bimetallic mixed liquor |
| CN109486424A (en) * | 2018-10-22 | 2019-03-19 | 安徽青润精密科技有限公司 | A kind of handware process of surface treatment |
| CN110484855A (en) * | 2019-09-26 | 2019-11-22 | 中国人民解放军陆军装甲兵学院 | A kind of erosion resistant, the supersonic speed plasma Ni base spray coating preparation method of excellent fatigue property |
| CN111168182A (en) * | 2020-01-06 | 2020-05-19 | 中航力源液压股份有限公司 | Preparation method of intermediate transition layer applied to vacuum diffusion welding |
| CN111378942A (en) * | 2018-12-28 | 2020-07-07 | 芜湖美的厨卫电器制造有限公司 | Anti-corrosion treatment process for metal surface, metal workpiece, electric heating pipe and electric water heater |
| CN111748763A (en) * | 2019-03-26 | 2020-10-09 | Oppo广东移动通信有限公司 | Method for enhancing adsorption capacity of stainless steel by magnet, supporting device and electronic equipment |
| CN111962123A (en) * | 2020-08-21 | 2020-11-20 | 马鞍山市小沈车行 | Surface treatment method of aluminum alloy wear-resistant part, internal combustion engine piston and application of internal combustion engine piston |
| CN112795886A (en) * | 2020-12-24 | 2021-05-14 | 上海治臻新能源装备有限公司 | Conductive corrosion-resistant precoating for forming metal bipolar plate and preparation method thereof |
| CN113067007A (en) * | 2021-03-19 | 2021-07-02 | 哈尔滨工业大学（深圳） | Solid fuel cell composite sealing layer and preparation method thereof |
| CN114086122A (en) * | 2021-11-26 | 2022-02-25 | 江苏科技大学 | Ceramic-based gradient plating layer based on high film-substrate binding force on copper substrate and preparation method thereof |
| CN114351081A (en) * | 2022-01-12 | 2022-04-15 | 江西瑞鼎精密传动有限公司 | Machining method of wear-resistant gear for miniature speed reducer |
| CN114713754A (en) * | 2022-04-13 | 2022-07-08 | 山东大学 | Surface coating, preparation method thereof, coating tool and bevel gear precision forging die |
| CN115161598A (en) * | 2021-04-06 | 2022-10-11 | 中山鼎兴真空科技有限公司 | Method for treating surface of club head |
| CN115341169A (en) * | 2021-05-14 | 2022-11-15 | 北京小米移动软件有限公司 | Surface treatment method |
| CN115336845A (en) * | 2021-05-14 | 2022-11-15 | 北京小米移动软件有限公司 | Terminal device |
| CN116145077A (en) * | 2023-04-19 | 2023-05-23 | 艾瑞森表面技术（苏州）股份有限公司 | Ion nitriding method for PVD (physical vapor deposition) pre-precipitation and composite coating |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH03277766A (en) * | 1990-03-28 | 1991-12-09 | Sumitomo Metal Ind Ltd | Black surface treated steel sheet and its production |
| JP2004283995A (en) * | 2003-03-25 | 2004-10-14 | Nachi Fujikoshi Corp | Advanced high-speed steel tool |
-
2014
- 2014-01-16 CN CN201410018736.1A patent/CN103805996B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH03277766A (en) * | 1990-03-28 | 1991-12-09 | Sumitomo Metal Ind Ltd | Black surface treated steel sheet and its production |
| JP2004283995A (en) * | 2003-03-25 | 2004-10-14 | Nachi Fujikoshi Corp | Advanced high-speed steel tool |
Non-Patent Citations (2)
| Title |
|---|
| H.C.MAN ET AL.: "In situ formation of a TiN/Ti metal matrix composite gradient coating on NiTi by laser cladding and nitriding", 《SURFACE & COATINGS TECHNOLOGY》 * |
| 赵彦辉 等: "等离子体氮化与物理气相沉积复合处理的研究进展", 《机械工程材料》 * |
Cited By (30)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104561909A (en) * | 2015-01-27 | 2015-04-29 | 大连理工常州研究院有限公司 | Ionitriding/arc ion plating surface composite modification apparatus and method |
| CN104947143A (en) * | 2015-05-29 | 2015-09-30 | 华北水利水电大学 | Titanium-based TiNx/TiO2-RuO2 coating anode |
| RU2611003C1 (en) * | 2015-11-02 | 2017-02-17 | Федеральное государственное бюджетное образовательное учреждение высшего профессионального образования "Уфимский государственный авиационный технический университет" | Method of ion nitration of titanium alloys |
| RU2625518C2 (en) * | 2015-11-02 | 2017-07-14 | Федеральное государственное бюджетное образовательное учреждение высшего профессионального образования "Уфимский государственный авиационный технический университет" | Method of nitridation of titanic alloys in glow discharge |
| CN105349941A (en) * | 2015-11-16 | 2016-02-24 | 哈尔滨工业大学 | Modification method for obtaining high-harness and high-wear-resistance gradient layer on surface of copper alloy |
| CN105568211A (en) * | 2015-12-29 | 2016-05-11 | 哈尔滨工业大学 | Method for enhancing diffusion of plasma on aluminum alloy surface |
| CN105568211B (en) * | 2015-12-29 | 2018-09-07 | 哈尔滨工业大学 | A kind of method that reinforcing is oozed in aluminum alloy surface plasma expansion |
| CN105908119A (en) * | 2016-04-23 | 2016-08-31 | 上海大学 | Surface oxidation treatment method of aluminum alloy extrusion die |
| CN108247191A (en) * | 2016-12-29 | 2018-07-06 | 核工业西南物理研究院 | A kind of method that hot isostatic pressing prevents welding assembly and jacket adhesion |
| CN107937876A (en) * | 2017-12-29 | 2018-04-20 | 中国电子科技集团公司第四十三研究所 | A kind of TiAlN composite superhard coatings with the support of hardness gradient layer and preparation method thereof |
| CN108372281A (en) * | 2018-03-28 | 2018-08-07 | 北京鼎翰科技有限公司 | A kind of tubing casting method based on stainless steel and carbon steel bimetallic mixed liquor |
| CN109486424A (en) * | 2018-10-22 | 2019-03-19 | 安徽青润精密科技有限公司 | A kind of handware process of surface treatment |
| CN111378942A (en) * | 2018-12-28 | 2020-07-07 | 芜湖美的厨卫电器制造有限公司 | Anti-corrosion treatment process for metal surface, metal workpiece, electric heating pipe and electric water heater |
| CN111748763A (en) * | 2019-03-26 | 2020-10-09 | Oppo广东移动通信有限公司 | Method for enhancing adsorption capacity of stainless steel by magnet, supporting device and electronic equipment |
| CN110484855A (en) * | 2019-09-26 | 2019-11-22 | 中国人民解放军陆军装甲兵学院 | A kind of erosion resistant, the supersonic speed plasma Ni base spray coating preparation method of excellent fatigue property |
| CN111168182A (en) * | 2020-01-06 | 2020-05-19 | 中航力源液压股份有限公司 | Preparation method of intermediate transition layer applied to vacuum diffusion welding |
| CN111168182B (en) * | 2020-01-06 | 2022-03-01 | 中航力源液压股份有限公司 | Preparation method of intermediate transition layer applied to vacuum diffusion welding |
| CN111962123A (en) * | 2020-08-21 | 2020-11-20 | 马鞍山市小沈车行 | Surface treatment method of aluminum alloy wear-resistant part, internal combustion engine piston and application of internal combustion engine piston |
| CN112795886A (en) * | 2020-12-24 | 2021-05-14 | 上海治臻新能源装备有限公司 | Conductive corrosion-resistant precoating for forming metal bipolar plate and preparation method thereof |
| CN113067007A (en) * | 2021-03-19 | 2021-07-02 | 哈尔滨工业大学（深圳） | Solid fuel cell composite sealing layer and preparation method thereof |
| CN115161598A (en) * | 2021-04-06 | 2022-10-11 | 中山鼎兴真空科技有限公司 | Method for treating surface of club head |
| CN115336845A (en) * | 2021-05-14 | 2022-11-15 | 北京小米移动软件有限公司 | Terminal device |
| CN115341169A (en) * | 2021-05-14 | 2022-11-15 | 北京小米移动软件有限公司 | Surface treatment method |
| CN114086122A (en) * | 2021-11-26 | 2022-02-25 | 江苏科技大学 | Ceramic-based gradient plating layer based on high film-substrate binding force on copper substrate and preparation method thereof |
| CN114086122B (en) * | 2021-11-26 | 2023-06-20 | 江苏科技大学 | Ceramic-based gradient plating layer based on high film-based binding force on copper substrate and preparation method thereof |
| CN114351081A (en) * | 2022-01-12 | 2022-04-15 | 江西瑞鼎精密传动有限公司 | Machining method of wear-resistant gear for miniature speed reducer |
| CN114351081B (en) * | 2022-01-12 | 2023-11-07 | 江西瑞鼎精密传动有限公司 | Processing method of wear-resistant gear for miniature speed reducer |
| CN114713754A (en) * | 2022-04-13 | 2022-07-08 | 山东大学 | Surface coating, preparation method thereof, coating tool and bevel gear precision forging die |
| CN116145077A (en) * | 2023-04-19 | 2023-05-23 | 艾瑞森表面技术（苏州）股份有限公司 | Ion nitriding method for PVD (physical vapor deposition) pre-precipitation and composite coating |
| CN116145077B (en) * | 2023-04-19 | 2023-08-08 | 艾瑞森表面技术（苏州）股份有限公司 | Ion nitriding method for PVD (physical vapor deposition) pre-precipitation and composite coating |
Also Published As
| Publication number | Publication date |
|---|---|
| CN103805996B (en) | 2015-09-16 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN103805996B (en) | The compounding method of the first plated film of a kind of metal material surface nitriding again | |
| US9133543B2 (en) | Coating material for aluminum die casting mold and method for manufacturing the same | |
| CN106222610B (en) | A kind of nanometer composite hard coating and preparation method thereof | |
| CN104911552B (en) | Method for reinforcing surface of hot-extrusion die through cementation compounding | |
| CN102392246B (en) | Metal surface treatment process | |
| CN102912298B (en) | Cr-doped DLC (diamond-like carbon) coating with anticorrosion and antifriction properties and preparation method | |
| CN102925862B (en) | Preparation method of Ti-doped diamond-like carbon (DLC) coating | |
| CN105132876B (en) | A kind of surface recombination processing method of steel gear | |
| CN104561910A (en) | Plasma enhanced arc ion plating equipment and method for preparing precision coating | |
| CN101698363B (en) | TiN/(TiN+CrN)/CrAlN nano composite coating and preparation method thereof | |
| CN103451608A (en) | Wolframium (W) doped diamond-like coating and preparation method thereof | |
| CN107338409B (en) | Process method for preparing nitrogen-based hard coating by adjustable magnetic field arc ion plating | |
| US20160186306A1 (en) | TiB2 LAYERS AND MANUFACTURE THEREOF | |
| CN110724923A (en) | Preparation method of ion-impregnated tungsten carbide layer with surface gradient nanostructure | |
| CN106884136A (en) | A kind of metal material surface nitriding deposits the wear-resisting modified layer preparation method of duplex anti-friction | |
| TW201339331A (en) | Coated article and method for making same | |
| CN114351110B (en) | Reinforced diamond-like film and preparation method thereof | |
| CN107675136B (en) | A kind of method of workpiece surface PVD plated film | |
| CN204434722U (en) | A kind of plasma enhancing prepares the arc ion plating apparatus of fine layers | |
| CN108265271A (en) | A kind of method that physical vaporous deposition makes blue film on product | |
| TW201251566A (en) | Housing and method for making same | |
| US20200199734A1 (en) | Magnesium alloy surface coating method and corrosion-resistant magnesium alloy prepared thereby | |
| RU2566232C1 (en) | Method of combined ion-plasma treatment of products out of aluminium alloys | |
| RU2515714C1 (en) | Method of nanocomposite coating application onto steel article surface | |
| CN106637077A (en) | Preparation method of tool surface coating and prepared coating |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant |