CN110373519A - A kind of preparation method of the stainless steel of high-hardness wear-resistant - Google Patents

A kind of preparation method of the stainless steel of high-hardness wear-resistant Download PDF

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CN110373519A
CN110373519A CN201910627542.4A CN201910627542A CN110373519A CN 110373519 A CN110373519 A CN 110373519A CN 201910627542 A CN201910627542 A CN 201910627542A CN 110373519 A CN110373519 A CN 110373519A
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ion
stainless steel
arc
film layer
matrix
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CN110373519B (en
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徐照英
肖艳红
苏永要
张腾飞
王锦标
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Shenzhen Hongyue Information Technology Co ltd
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Chongqing University of Arts and Sciences
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    • CCHEMISTRY; METALLURGY
    • C21METALLURGY OF IRON
    • C21DMODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
    • C21D1/00General methods or devices for heat treatment, e.g. annealing, hardening, quenching or tempering
    • C21D1/18Hardening; Quenching with or without subsequent tempering
    • CCHEMISTRY; METALLURGY
    • C23COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23CCOATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/0021Reactive sputtering or evaporation
    • CCHEMISTRY; METALLURGY
    • C23COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23CCOATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/02Pretreatment of the material to be coated
    • C23C14/021Cleaning or etching treatments
    • CCHEMISTRY; METALLURGY
    • C23COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23CCOATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/06Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
    • C23C14/0641Nitrides
    • CCHEMISTRY; METALLURGY
    • C23COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23CCOATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/22Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
    • C23C14/24Vacuum evaporation
    • C23C14/32Vacuum evaporation by explosion; by evaporation and subsequent ionisation of the vapours, e.g. ion-plating
    • C23C14/325Electric arc evaporation
    • CCHEMISTRY; METALLURGY
    • C23COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23CCOATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/22Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
    • C23C14/48Ion implantation
    • CCHEMISTRY; METALLURGY
    • C23COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23GCLEANING OR DE-GREASING OF METALLIC MATERIAL BY CHEMICAL METHODS OTHER THAN ELECTROLYSIS
    • C23G1/00Cleaning or pickling metallic material with solutions or molten salts
    • C23G1/02Cleaning or pickling metallic material with solutions or molten salts with acid solutions
    • C23G1/08Iron or steel
    • C23G1/088Iron or steel solutions containing organic acids
    • CCHEMISTRY; METALLURGY
    • C23COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23GCLEANING OR DE-GREASING OF METALLIC MATERIAL BY CHEMICAL METHODS OTHER THAN ELECTROLYSIS
    • C23G1/00Cleaning or pickling metallic material with solutions or molten salts
    • C23G1/14Cleaning or pickling metallic material with solutions or molten salts with alkaline solutions
    • C23G1/19Iron or steel

Abstract

The present invention provides a kind of preparation method of the stainless steel of high-hardness wear-resistant, its step specifically includes: being machined, is heat-treated to matrix first, polished and polishing treatment, then it cleaned, dried, the ion implanting of titanium and nitrogen dual element is carried out using ion implantation, then the depositing Ti AlN film layer in multi-Arc Ion Plating, then VN film layer is deposited in multi-Arc Ion Plating.The stainless steel that the present invention prepares hardness with higher, good machinability, electric conductivity, thermal conductivity etc., while the functional complete, high yield rate of the method for the present invention condition controllable precise, stainless steel watch finishing coat.

Description

A kind of preparation method of the stainless steel of high-hardness wear-resistant
Technical field
The present invention relates to a kind of technical field of alloy steel, and in particular to a kind of stainless steel of high-hardness wear-resistant.
Background technique
Stainless steel refers to the steel of the chemical etchings dielectric corrosions such as the weak corrosive medium such as resistance to air, steam, water and acid, alkali, salt, Also known as stainless acid resistant steel.In practical application, often the steel by resistance to weak corrosive medium corrosion is known as stainless steel, and resistant to chemical media is rotten The steel of erosion is known as acid resisting steel.Due to difference of the two in chemical component, not necessarily resistant to chemical media corrodes for the former, and the latter is then Generally there is rustless property.The corrosion resistance of stainless steel depends on alloying element contained in steel.
In modern society, stainless steel has extremely extensive purposes, it not only can be applied in household products, but also can be used for In industrial production.As people are more and more widely used stainless steel, properties are also gradually increased.But current existing skill In art, still not publicly realized for the high-temperature machinery of representative, requirement from room temperature for some such as all kinds of high-performance aeroengines To continuously running as the stainless steel in the high tech equipments fields such as the geological drilling field of representative for high temperature because its hardness with it is wear-resisting The requirement of high-strength working is not achieved in performance.Therefore, prepare that a kind of hardness is high, fusing point is high, stability is good, coefficient of friction is low not Rust steel will be an important technological means in industrial production from now on.
By the patent of 104520472 A of application publication number CN it is found that TiAlN has high hardness, height as coating Elasticity modulus;By the patent of 103726014 A of application publication number CN it is found that VN is as coating, mill high with abrasive resistance The inefficient fruit of loss rate.But due to low etc. in the presence of very big internal stress, adhesiveness between TiAlN and VN combination painting interlayer, coating and matrix Problem, the problem of layering occurs so as to cause film, peels off and fails;So still not publicly being combined at present using TiAlN and VN Composite coating, make stainless steel surface that there is the characteristic of high rigidity, self-lubricating (i.e. abrasive resistance high).
Summary of the invention
For the above technical problem, it is an object of that present invention to provide a kind of preparation sides of the stainless steel of high-hardness wear-resistant Method, the stainless steel hardness prepared is high, fusing point is high, stability is good, coefficient of friction is low, is applicable to aero-engine, geology Drill contour strength fields.
The object of the invention is achieved through the following technical solutions:
A kind of preparation method of the stainless steel of high-hardness wear-resistant, selection stainless steel are basis material, which is characterized in that it Through the following steps that carrying out: being machined, be heat-treated to matrix first, polished and polishing treatment, then carried out clear It washes, dry, the ion implanting of titanium and nitrogen dual element is carried out using ion implantation, is then deposited in multi-Arc Ion Plating TiAlN film layer, then VN film layer is deposited in multi-Arc Ion Plating.
The stainless steel that high-hardness wear-resistant is prepared using above-mentioned steps is effectively reduced the internal stress of film and matrix, mentioned High binding force between film and matrix avoids film that layering occurs, peels off and the problems such as failure, guarantee prepares high hardness wear-resisting The yield rate of the stainless steel of damage.
Further, above-mentioned heat treatment need to carry out 1240 DEG C of high temperature quenchings and three times 560 DEG C of high temperings;The polishing exists It is carried out on grinding machine, successively uses 800#, 1000#, 1500# liquid honing;The polishing treatment carries out on polishing machine, uses grain The diamond that diameter is 0.1 μm is as polishing agent.
Further, above-mentioned cleaning uses Acid-Base treatment fluid, first carries out alkali process, then carry out sour processing.
In using the preprocessing process before ion implanting, if matrix surface there are scratch or matrix hardness are lower, carries out Acid-Base treatment fluid processing when, Acid-Base treatment fluid can react with matrix surface, thus influence subsequent ion injection and it is thin Film deposition.Using step combination of the invention and treatment process, ensure matrix surface in the case where guaranteeing matrix hardness Smooth degree guarantees after pretreatment that ion implanting and film deposit and goes on smoothly, so that it is guaranteed that prepare film condition controllable precise, Film is fully functional.
Further, above-mentioned ion implantation uses metal vapor vacuum arc (Metal Vapor Vacuum Arc, MEVVA) Ion implantation apparatus;Above-mentioned ion implantation be using high purity titanium as target and be passed through nitrogen progress titanium and nitrogen dual element ion Injection.
Further, the energy of above-mentioned ion implantation Ti ion are as follows: the projected range Rp and range of 45-50keV, Ti ion Straggling is 45.1,16.5nm, and the implantation dosage of Ti ion is fixed are as follows: 1.0 × 1017-1.5×1017ions/cm2;N ion implanting Parameter are as follows: vacuum chamber background vacuum 1.0x10-3Pa, N20.6-0.9Pa is divided, applies the inclined of -2.5~-2.0kV on matrix Pressure, frequency 16-20kHz, N ion implanting time are 2.5-3.5h;It injects during Ti ion, incident ion is stainless with substrate Steel surface keeps 90 ° of angles, and beam intensity is controlled in 4.0-4.5A/cm2, increased to avoid temperature caused by ion implantation process Effect;It injects during N ion, N ion vertical incidence.
When using ion implantation, due to ion motion trace unstability and ion incidence matrix surface when generate Impact, cause ion implanting matrix to there is the technical problem reunited, when preparing plural layers so as to cause subsequent step Failure or it is uneven, preparation yield rate is not high, while also will affect the binding force of matrix Yu each layer film;Using place of the invention Science and engineering skill and step combination, it is ensured that dispersibility and uniformity when ion implanting, it is ensured that subsequent step is gone on smoothly, and is guaranteed Bond strength between the uniformity of film, yield rate and matrix and film.
Further, above-mentioned multi-Arc Ion Plating uses WH-800 type multi-Arc Ion Plating, main coating process Parameter is depositing temperature: 450-500 DEG C, nitrogen partial pressure: and 0.8-1.0Pa, flow: 80sccm, arc current: 80-90A, negative voltage :- 220~-180V, vacuum degree: 4 × 10-3Pa, plated film time: 60-80min.
Further, the above-mentioned depositing Ti AlN film layer in multi-Arc Ion Plating is using high purity titanium and rafifinal as target, And it is passed through nitrogen;VN film layer is deposited in multi-Arc Ion Plating using high purity vanadium as target, and is passed through nitrogen.
Further, TiAlN film layer obtained above is 110nm-130nm;VN film layer is 120nm-140nm.
A kind of stainless steel of high-hardness wear-resistant and preparation method thereof, which is characterized in that it is through the following steps that carry out:
A, it selects stainless steel as basis material, machining appropriate is carried out to basis material, becomes and meets work Industry uses the tool or mold shape of standard;Then matrix is carried out carrying out 1240 DEG C of high temperature quenchings and three times 560 DEG C of high temperature The heat treatment of tempering is successively polished with 800#, 1000#, 1500# waterproof abrasive paper on grinding machine, the gold for the use of partial size being 0.1 μm Hard rock is processed by shot blasting on polishing machine as polishing agent;
B, the mixed solvents such as tap water, alcohol, Acid-Base treatment fluid, high purity water-are successively carried out to tool or die matrix The cleaning of the multisteps such as ultrasonic wave, acetone-ultrasonic wave and pretreatment, then dry, spare;Wherein soda acid treatment fluid is respectively HF+HN O3+ HAC (molar ratio 1: 1: 1) mixed acid and K3(Fe(CN)6)+KOH (mass ratio 1: 1) mixed ammonium/alkali solutions, and first carry out alkali process Surface roughening is carried out to basis material, then carries out the impurity that acid processing removes matrix surface;
C, the matrix after pretreatment and cleaning is put into the flood chamber of ion implantation apparatus, flood chamber is first evacuated to vacuum shape State using titanium target and injects nitrogen and carries out titanium and nitrogen dual element using injecting 3~10min of element target needed for argon purge Ion implanting processing;Wherein, the energy of Ti ion are as follows: the projected range Rp and range straggling of 45-50keV, Ti ion be 45.1, The implantation dosage of 16.5nm, Ti ion is fixed are as follows: 1.0 × 1017-1.5×1017ions/cm2;N ion implanting parameter are as follows: vacuum Room background vacuum 1.0x10-3Pa, N20.6-0.9Pa is divided, applies the bias of -2.5~-2.0kV on matrix, frequency is 16-20kHz, N the ion implanting time are 2.5-3.5h;It injects during Ti ion, incident ion and substrate stainless steel surface are protected 90 ° of angles are held, beam intensity is controlled in 4.0-4.5A/cm2, effect is increased to avoid temperature caused by ion implantation process;Note During entering N ion, N ion vertical incidence;
D, the matrix after injection ion is put into multi-Arc Ion Plating, first with Nitrogen ion Bombardment and cleaning adsorption Impurity recycles titanium, aluminium as target, and arc erosion generates N3-、Al3+、Ti2+Ion, these ions act in back bias voltage Product obtains certain thickness film as high rigidity surface layer;Wherein, using WH-800 type multi-Arc Ion Plating, coating process ginseng Number is depositing temperature: 450-500 DEG C, nitrogen partial pressure: 0.8-1.0Pa, flow: 80sccm, arc current: 80-90A, negative voltage: -220 ~-180V, vacuum degree: 4 × 10-3Pa, plated film time: 60-80min;
E, the matrix for having high rigidity surface layer is put into multi-Arc Ion Plating, is passed through nitrogen, is target, electric arc using vanadium Ablation generates N3-、V3+, these ions back bias voltage effect under deposition obtain certain thickness film as self-lubricating surface layer;Its In, using WH-800 type multi-Arc Ion Plating, coating process parameter is depositing temperature: 450-500 DEG C, nitrogen partial pressure: 0.8- 1.0Pa, flow: 80sccm, arc current: 80-90A, negative voltage: -220~-180V, vacuum degree: 4 × 10-3Pa, plated film time: 60-80min。
The present invention has the following technical effect that:
The present invention provides a kind of preparation method of the stainless steel of high-hardness wear-resistant so that the stainless steel prepared have compared with High hardness, good machinability, electric conductivity, thermal conductivity etc.;It is but also with ceramic characteristics, such as higher springform simultaneously Amount, good corrosion resistance and high temperature oxidation resistance etc..Meanwhile the stainless steel of high-hardness wear-resistant is prepared using this method, The functional complete, high yield rate of condition controllable precise, stainless steel watch finishing coat, solves its hardness as caused by coating film treatment Elasticity modulus reduces, rub secondary lubrication under different condition;Also solve the problems, such as that ion is reunited when ion implanting, it is ensured that thin Bond strength between the uniformity and matrix and film of film.
Detailed description of the invention
Fig. 1 is stainless steel surface cross-sectional view obtained in the embodiment of the present invention 1.
Fig. 2 is the shape appearance figure of stainless steel and SiC ball opposite grinding obtained in the embodiment of the present invention 2.
Fig. 3 is the impression figure of stainless steel binding force test obtained in the embodiment of the present invention 3.
Fig. 4 is the scratch figure of stainless steel binding force test obtained in the embodiment of the present invention 3.
Wherein, figure (a) is scratch exterior view, and figure (b) is electron microscope.
Specific embodiment
In order to make the object, technical scheme and advantages of the embodiment of the invention clearer, below in conjunction with the embodiment of the present invention In attached drawing, technical solution in the embodiment of the present invention is explicitly described, it is clear that described embodiment is the present invention A part of the embodiment, instead of all the embodiments.
Embodiment 1
A kind of preparation method of the stainless steel of high-hardness wear-resistant, selection grade of steel are Cr25Mo3Ti, having a size of 60x60mm's Stainless steel is basis material, it is characterised in that:
It a, is Cr to grade of steel25Mo3Ti, the stainless steel base material having a size of 60x60mm carry out machining appropriate, make It becomes the tool or mold shape for meeting industrial application standard;Then matrix is carried out carrying out 1240 DEG C of high temperature quenchings and three The heat treatment of secondary 560 DEG C of high temperings, is successively polished with 800#, 1000#, 1500# waterproof abrasive paper on grinding machine, uses partial size Diamond for 0.1 μm is processed by shot blasting on polishing machine as polishing agent;
B, the mixed solvents such as tap water, alcohol, Acid-Base treatment fluid, high purity water-are successively carried out to tool or die matrix The cleaning of the multisteps such as ultrasonic wave, acetone-ultrasonic wave and pretreatment, then dry, spare;Wherein soda acid treatment fluid is respectively HF+HN O3+ HAC (molar ratio 1: 1: 1) mixed acid and K3(Fe(CN)6)+KOH (mass ratio 1: 1) mixed ammonium/alkali solutions, and first carry out alkali process Surface roughening is carried out to basis material, then carries out the impurity that acid processing removes matrix surface;
C, the matrix after pretreatment and cleaning is put into the flood chamber of ion implantation apparatus, flood chamber is first evacuated to vacuum shape State using titanium target and injects nitrogen and carries out titanium and nitrogen dual element using injecting 3~10min of element target needed for argon purge Ion implanting processing;Wherein, the energy of Ti ion are as follows: the projected range Rp and range straggling of 45ke V, Ti ion be 45.1, The implantation dosage of 16.5nm, Ti ion is fixed are as follows: 1.0 × 1017ions/cm2;N ion implanting parameter are as follows: vacuum chamber base vacuum Spend 1.0x10-3Pa, N20.6Pa is divided, the bias of application -2.0kV on matrix, frequency 16kHz, N the ion implanting time is 2.5h;It injects during Ti ion, incident ion and substrate stainless steel surface keep 90 ° of angles, and beam intensity is controlled in 4.0A/ cm2, effect is increased to avoid temperature caused by ion implantation process;It injects during N ion, N ion vertical incidence;
D, the matrix after injection ion is put into multi-Arc Ion Plating, first with Nitrogen ion Bombardment and cleaning adsorption Impurity recycles titanium, aluminium as target, and arc erosion generates N3-、Al3+、Ti2+Ion, these ions act in back bias voltage Product obtains the film with a thickness of 110nm as high rigidity surface layer;Wherein, using WH-800 type multi-Arc Ion Plating, plated film work Skill parameter is depositing temperature: 450 DEG C, nitrogen partial pressure: 0.8Pa, flow: 80sccm, arc current: 80A, negative voltage: -180V, vacuum Degree: 4 × 10-3Pa, plated film time: 60min;
E, the matrix for having high rigidity surface layer is put into multi-Arc Ion Plating, is passed through nitrogen, is target, electric arc using vanadium Ablation generates N3-、V3+, these ions back bias voltage effect under deposition obtain the film with a thickness of 120nm as self-lubricating surface layer; Wherein, using WH-800 type multi-Arc Ion Plating, coating process parameter is depositing temperature: 450 DEG C, nitrogen partial pressure: 0.8Pa, stream Amount: 80sccm, arc current: 80A, negative voltage: -180V, vacuum degree: 4 × 10-3Pa, plated film time: 60min.
Embodiment 2
A kind of preparation method of the stainless steel of high-hardness wear-resistant, selection grade of steel are Cr17Mo2Ti, having a size of 80x80mm's Stainless steel is basis material, it is characterised in that:
It a, is Cr to matrix number17Mo2Ti, the stainless steel material having a size of 80x80mm carry out machining appropriate, make it As the tool or mold shape for meeting industrial application standard;Then carry out 1240 DEG C of high temperature quenching and three times to matrix The heat treatment of 560 DEG C of high temperings, is successively polished with 800#, 1000#, 1500# waterproof abrasive paper on grinding machine, is using partial size 0.1 μm of diamond is processed by shot blasting on polishing machine as polishing agent;
B, the mixed solvents such as tap water, alcohol, Acid-Base treatment fluid, high purity water-are successively carried out to tool or die matrix The cleaning of the multisteps such as ultrasonic wave, acetone-ultrasonic wave and pretreatment, then dry, spare;Wherein soda acid treatment fluid is respectively HF+HN O3+ HAC (molar ratio 1: 1: 1) mixed acid and K3(Fe(CN)6)+KOH (mass ratio 1: 1) mixed ammonium/alkali solutions, and first carry out alkali process Surface roughening is carried out to basis material, then carries out the impurity that acid processing removes matrix surface;
C, the matrix after pretreatment and cleaning is put into the flood chamber of ion implantation apparatus, flood chamber is first evacuated to vacuum shape State using titanium target and injects nitrogen and carries out titanium and nitrogen dual element using injecting 3~10min of element target needed for argon purge Ion implanting processing;Wherein, the energy of Ti ion are as follows: the projected range Rp and range straggling of 47ke V, Ti ion be 45.1, The implantation dosage of 16.5nm, Ti ion is fixed are as follows: 1.2 × 1017ions/cm2;N ion implanting parameter are as follows: vacuum chamber base vacuum Spend 1.0x10-3Pa, N20.75Pa is divided, the bias of application -2.2kV on matrix, frequency 18kHz, N the ion implanting time is 3.0h;It injects during Ti ion, incident ion and substrate stainless steel surface keep 90 ° of angles, and beam intensity is controlled in 4.2A/ cm2, effect is increased to avoid temperature caused by ion implantation process;It injects during N ion, N ion vertical incidence;
D, the matrix after injection ion is put into multi-Arc Ion Plating, first with Nitrogen ion Bombardment and cleaning adsorption Impurity recycles titanium, aluminium as target, and arc erosion generates N3-、Al3+、Ti2+Ion, these ions act in back bias voltage Product obtains the film with a thickness of 120nm as high rigidity surface layer;Wherein, using WH-800 type multi-Arc Ion Plating, plated film work Skill parameter is depositing temperature: 475 DEG C, nitrogen partial pressure: 0.9Pa, flow: 80sccm, arc current: 85A, negative voltage: -200V, vacuum Degree: 4 × 10-3Pa, plated film time: 70min;
E, the matrix for having high rigidity surface layer is put into multi-Arc Ion Plating, is passed through nitrogen, is target, electric arc using vanadium Ablation generates N3-、V3+, these ions back bias voltage effect under deposition obtain the film with a thickness of 130nm as self-lubricating surface layer; Wherein, using WH-800 type multi-Arc Ion Plating, coating process parameter is depositing temperature: 475 DEG C, nitrogen partial pressure: 0.9Pa, stream Amount: 80sccm, arc current: 85A, negative voltage: -200V, vacuum degree: 4 × 10-3Pa, plated film time: 70min.
Embodiment 3
A kind of preparation method of the stainless steel of high-hardness wear-resistant, the selection trade mark are 0Cr19Ni9, having a size of 60x70mm's Stainless steel is basis material, it is characterised in that:
It a, is 0Cr to the trade mark19Ni9, stainless steel base material having a size of 60x70mm carry out machining appropriate, make It becomes the tool or mold shape for meeting industrial application standard;Then matrix is carried out carrying out 1240 DEG C of high temperature quenchings and three The heat treatment of secondary 560 DEG C of high temperings, is successively polished with 800#, 1000#, 1500# waterproof abrasive paper on grinding machine, uses partial size Diamond for 0.1 μm is processed by shot blasting on polishing machine as polishing agent;
B, the mixed solvents such as tap water, alcohol, Acid-Base treatment fluid, high purity water-are successively carried out to tool or die matrix The cleaning of the multisteps such as ultrasonic wave, acetone-ultrasonic wave and pretreatment, then dry, spare;Wherein soda acid treatment fluid is respectively HF+HN O3+ HAC (molar ratio 1: 1: 1) mixed acid and K3(Fe(CN)6)+KOH (mass ratio 1: 1) mixed ammonium/alkali solutions, and first carry out alkali process Surface roughening is carried out to basis material, then carries out the impurity that acid processing removes matrix surface;
C, the matrix after pretreatment and cleaning is put into the flood chamber of ion implantation apparatus, flood chamber is first evacuated to vacuum shape State using titanium target and injects nitrogen and carries out titanium and nitrogen dual element using injecting 3~10min of element target needed for argon purge Ion implanting processing;Wherein, the energy of Ti ion are as follows: the projected range Rp and range straggling of 50ke V, Ti ion be 45.1, The implantation dosage of 16.5nm, Ti ion is fixed are as follows: 1.5 × 1017ions/cm2;N ion implanting parameter are as follows: vacuum chamber base vacuum Spend 1.0x10-3Pa, N20.9Pa is divided, the bias of application -2.5kV on matrix, frequency 20kHz, N the ion implanting time is 3.5h;It injects during Ti ion, incident ion and substrate stainless steel surface keep 90 ° of angles, and beam intensity is controlled in 4.5A/ cm2, effect is increased to avoid temperature caused by ion implantation process;It injects during N ion, N ion vertical incidence;
D, the matrix after injection ion is put into multi-Arc Ion Plating, first with Nitrogen ion Bombardment and cleaning adsorption Impurity recycles titanium, aluminium as target, and arc erosion generates N3-、Al3+、Ti2+Ion, these ions act in back bias voltage Product obtains the film with a thickness of 130nm as high rigidity surface layer;Wherein, using WH-800 type multi-Arc Ion Plating, plated film work Skill parameter is depositing temperature: 500 DEG C, nitrogen partial pressure: 1.0Pa, flow: 80sccm, arc current: 90A, negative voltage: -220V, vacuum Degree: 4 × 10-3Pa, plated film time: 80min;
E, the matrix for having high rigidity surface layer is put into multi-Arc Ion Plating, is passed through nitrogen, is target, electric arc using vanadium Ablation generates N3-、V3+, these ions back bias voltage effect under deposition obtain the film with a thickness of 140nm as self-lubricating surface layer; Wherein, using WH-800 type multi-Arc Ion Plating, coating process parameter is depositing temperature: 500 DEG C, nitrogen partial pressure: 1.0Pa, stream Amount: 80sccm, arc current: 90A, negative voltage: -220V, vacuum degree: 4 × 10-3Pa, plated film time: 80min.
Stainless steel obtained by embodiment 1-3 carries out micro-hardness testing, hard using DUH-211S Shimadzu dynamic submicroscopic Degree meter, pressure head are diamond micro Vickers pressure head, test load 10mN, maximum load retention time 5sec.Test result shows, The microhardness value of stainless steel is in 38-42GPa.
Fig. 1 is the cross-sectional view of high speed steel obtained in embodiment 1, as shown in Figure 1, prepared by the present invention hard Anti abrasive high-speed steel is spent, clear layer between surface layers, uniformly, each layer has the function of more complete.
Fig. 2 is the shape appearance figure of high speed steel and SiC ball opposite grinding obtained by embodiment 2, wherein load 3N, angle of rotation Speed is 95.49rmp, abrasion radius is 3.00mm, 50,000 turns of abrasion;Surface of high speed steel after experiment is without significant change, micro- The specific pattern of microscopic observation high-speed steel, as shown in Figure 2, surface of high speed steel is small by friction area, friction depth is shallow, it was demonstrated that high rigidity Anti abrasive high-speed steel shows good wear-resistant and wear-resisting property in an experiment, to prove that its self-lubricating effect is good.
Film substrate bond strength can qualitative or be semi-quantitatively evaluated by vickers indentation.This experiment is for made in embodiment 3 High speed steel, use Vickers indentation method apex angle for the tapered pressure head of 136 diamond, indentation test adopt the load of 3N into Row test.As seen from Figure 3, the high-speed steel after test integrally observe almost without crackle, only indentation edge have it is very slight Crackle does not occur any film separation phenomenon, shows preferable film-substrate cohesion.
Scratch experiment method be it is a kind of be widely used in measure ganoine thin film-basal body interface bond strength method of inspection.This Experiment uses pressure head for Ф 2 (mm) ball of GCr15 material for high speed steel obtained in embodiment 3, scratch experiment, Load is gradually increased to 100N by 0N, and scratch uses continuous loading method.Found out by Fig. 4 (a), it is whole in load 100N clearing end It is not peeled off during a load swiping, the scratch due to being plastically deformed generation on a small quantity only occurs, what film still maintained Extremely complete, this illustrates that film has excellent toughness and plasticity_resistant deformation ability, and plural layers have good intrinsic combination strong Degree and film-substrate cohesion.
Fig. 4 (b) is resulting HRTEM image, as can be seen that the area different in two layers of contrast from high resolution electron microscopy photo There is one layer of mixed zone between domain, brightness differentiation is unobvious, and it is very fuzzy, form apparent transitional region.The presence of transition region, can Effectively to enhance the binding characteristic between film layer.
Comprehensive Vickers indentation and scratch experiment as a result, bonding state has obtained a degree of change between film and matrix It is kind.It is multiple with dual extension-compression modulus layer formed composite constructions can Stopping cross section microcrack initiation, and then play improve film base The effect of binding force and the overall flexibility of plural layers.

Claims (5)

1. a kind of preparation method of the stainless steel of high-hardness wear-resistant, selection stainless steel is basis material, which is characterized in that it is It is carried out by following steps: matrix being machined first, is heat-treated, is polished and polishing treatment, then cleaned, It dries, the ion implanting of titanium and nitrogen dual element is carried out using ion implantation, then the depositing Ti AlN in multi-Arc Ion Plating Film layer, then VN film layer is deposited in multi-Arc Ion Plating.
2. a kind of preparation method of the stainless steel of high-hardness wear-resistant according to claim 1, it is characterised in that: the ion The energy of injection method Ti ion are as follows: the projected range Rp and range straggling of 45-50keV, Ti ion be 45.1,16.5nm, Ti from The implantation dosage of son is fixed are as follows: 1.0 × 1017-1.5×1017ions/cm2;N ion implanting parameter are as follows: vacuum chamber background vacuum 1.0x10-3Pa, N20.6-0.9Pa is divided, applies the bias of -2.5~-2.0kV, frequency 16-20kHz, N ion on matrix Injection length is 2.5-3.5h;It injects during Ti ion, incident ion and substrate stainless steel surface keep 90 ° of angles, line Strength control is in 4.0-4.5A/cm2, effect is increased to avoid temperature caused by ion implantation process;It injects during N ion, N Ion vertical incidence.
3. a kind of preparation method of the stainless steel of high-hardness wear-resistant according to claim 2, it is characterised in that: the multi sphere Ion plating equipment uses WH-800 type multi-Arc Ion Plating, and main coating process parameter is depositing temperature: 450-500 DEG C, nitrogen partial pressure: 0.8-1.0Pa, flow: 80sccm, arc current: 80-90A, negative voltage: -220~-180V, vacuum degree: 4 × 10-3Pa, plated film time: 60-80min.
4. a kind of preparation method of the stainless steel of high-hardness wear-resistant according to claim 3, it is characterised in that: described more Depositing Ti AlN film layer is using high purity titanium and rafifinal as target in arc ion plating equipment, and is passed through nitrogen;In multi-arc ion coating VN film layer is deposited in film machine using high purity vanadium as target, and is passed through nitrogen.
5. a kind of preparation method of the stainless steel of high-hardness wear-resistant according to claim 4, it is characterised in that: the above-mentioned system of institute The TiAlN film layer obtained is 110nm-130nm;VN film layer is 120nm-140nm.
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