CN110373637A - A kind of high speed steel and preparation method thereof - Google Patents

A kind of high speed steel and preparation method thereof Download PDF

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CN110373637A
CN110373637A CN201910627657.3A CN201910627657A CN110373637A CN 110373637 A CN110373637 A CN 110373637A CN 201910627657 A CN201910627657 A CN 201910627657A CN 110373637 A CN110373637 A CN 110373637A
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ion
speed steel
high speed
film layer
arc
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徐照英
邓川宁
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Chongqing University of Arts and Sciences
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    • C—CHEMISTRY; METALLURGY
    • C21—METALLURGY OF IRON
    • C21D—MODIFYING 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
    • C21D1/00—General methods or devices for heat treatment, e.g. annealing, hardening, quenching or tempering
    • C21D1/18—Hardening; Quenching with or without subsequent tempering
    • C—CHEMISTRY; METALLURGY
    • C23—COATING 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
    • C23C—COATING 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
    • C23C12/00—Solid state diffusion of at least one non-metal element other than silicon and at least one metal element or silicon into metallic material surfaces
    • C—CHEMISTRY; METALLURGY
    • C23—COATING 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
    • C23C—COATING 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
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/02—Pretreatment of the material to be coated
    • C23C14/021—Cleaning or etching treatments
    • C23C14/022—Cleaning or etching treatments by means of bombardment with energetic particles or radiation
    • C—CHEMISTRY; METALLURGY
    • C23—COATING 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
    • C23C—COATING 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
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
    • C23C14/0641—Nitrides
    • C—CHEMISTRY; METALLURGY
    • C23—COATING 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
    • C23C—COATING 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
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
    • C23C14/24—Vacuum evaporation
    • C23C14/32—Vacuum evaporation by explosion; by evaporation and subsequent ionisation of the vapours, e.g. ion-plating
    • C23C14/325—Electric arc evaporation
    • C—CHEMISTRY; METALLURGY
    • C23—COATING 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
    • C23G—CLEANING OR DE-GREASING OF METALLIC MATERIAL BY CHEMICAL METHODS OTHER THAN ELECTROLYSIS
    • C23G1/00—Cleaning or pickling metallic material with solutions or molten salts
    • C23G1/02—Cleaning or pickling metallic material with solutions or molten salts with acid solutions
    • C23G1/08—Iron or steel
    • C23G1/088—Iron or steel solutions containing organic acids
    • C—CHEMISTRY; METALLURGY
    • C23—COATING 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
    • C23G—CLEANING OR DE-GREASING OF METALLIC MATERIAL BY CHEMICAL METHODS OTHER THAN ELECTROLYSIS
    • C23G1/00—Cleaning or pickling metallic material with solutions or molten salts
    • C23G1/14—Cleaning or pickling metallic material with solutions or molten salts with alkaline solutions
    • C23G1/19—Iron or steel

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  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
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  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Physics & Mathematics (AREA)
  • Thermal Sciences (AREA)
  • Crystallography & Structural Chemistry (AREA)
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Abstract

The present invention provides a kind of high speed steel and preparation method thereof, its composite coating that TiAlN and VN are prepared in surface of high speed steel, specific steps include: to be machined, be 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 high-speed 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, surface of high speed steel coating.

Description

A kind of high speed steel and preparation method thereof
Technical field
The present invention relates to a kind of technical field of alloy steel, and in particular to a kind of high speed steel.
Background technique
High-speed steel (HSS) is a kind of tool steel with high rigidity, high-wearing feature and high-fire resistance, also known as high-speed tool steel Or high-speed steel, it is commonly called as Bai Gang.The processing performance of high-speed steel is good, and intensity and toughness are worked good, therefore is mainly used to the thin of manufacture complexity Sword and impact-resistant metal cutting tool, can also manufacture high-temperature bearing and cold extrusion die etc..Except the height produced with method of smelting Outside fast steel, occurs PM HSS after the 1960s again, its advantages are that of avoiding smelting process production and are made At carbide segregation and cause mechanical performance reduce and heat-treatment distortion.
In modern society, since high-speed steel has extensive use, people are also higher and higher to the performance requirement of high-speed steel.Mesh Although the high-speed steel in preceding industrial production has the advantages that hardness high, wearability and heat-resist, if being used for some high-tech Equipment field, such as all kinds of high-performance aeroengines are the high-temperature machinery of representative, require realization continuous from room temperature to high temperature Geological drilling field represented etc. is operated as, then its hardness and wearability are just unable to satisfy demand.Therefore, a kind of hardness is prepared High-speed steel high, that fusing point is high, stability is good, coefficient of friction is low will be an important technological means in industrial production from now on.
By the patent of application publication number CN 104520472A it is found that TiAlN is as coating, there is high hardness, high-elastic Property modulus；By the patent of application publication number CN 103726014A it is found that VN is as coating, the high, wear rate with abrasive resistance Inefficient fruit.But there is the problems such as very big internal stress, adhesiveness is low between interlayer, coating and matrix since TiAlN and VN combination applies, 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 compound Coating makes surface of high speed steel have the characteristic of high rigidity, self-lubricating (i.e. abrasive resistance is high).
Summary of the invention
For the above technical problem, it is an object of that present invention to provide a kind of high speed steel, hardness is high, fusing point is high, Stability is good, coefficient of friction is low, is applicable to the high strength fields such as aero-engine, geological drilling.
Another object of the present invention is to provide a kind of preparation methods of high speed steel, are used to prepare high hardness wear-resisting The high-speed steel of damage.
The object of the invention is achieved through the following technical solutions:
A kind of high speed steel, selection high-speed steel are basis material, which is characterized in that are followed successively by outward from matrix surface TiAlN film layer and VN film layer；The TiAlN thin film layer thickness is 80nm-100nm, and the VN thin film layer thickness is 80nm-100nm。
The above-mentioned high-speed steel as basis material can be that grade of steel is W2Mo9Cr4VCo8, grade of steel W6Mo5Cr4V2, grade of steel be W18Cr4V etc..
A kind of preparation method of high speed steel, selection regular high speed steels are basis material, which is characterized in that it is logical It crosses following steps progress: matrix being machined first, is heat-treated, is polished and polishing treatment, then being cleaned, dried in the air It is dry, the ion implanting of titanium and nitrogen dual element is carried out using ion implantation, then depositing Ti AlN is thin in multi-Arc Ion Plating Film layer, then VN film layer is deposited in multi-Arc Ion Plating.
High speed steel is prepared using above-mentioned steps, the internal stress of film and matrix is effectively reduced, improves film Binding force between matrix, the problems such as avoiding film that layering occurs, peel off and fail, guarantee prepares the finished product of high speed steel Rate.
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 40-45keV, Ti ion Straggling is 45.1,16.5nm, and the implantation dosage of Ti ion is fixed are as follows: 0.6 × 1017-1.0×1017ions/cm2；N ion implanting Parameter are as follows: vacuum chamber background vacuum 1.0x10-3Pa, N20.4-0.6Pa is divided, applies the inclined of -2.7~-2.5kV on matrix Pressure, frequency 14-16kHz, N ion implanting time are 2.0-3.0h；It injects during Ti ion, incident ion is stainless with substrate Steel surface keeps 90 ° of angles, and beam intensity is controlled in 3.7-4.0A/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: 430-470 DEG C, nitrogen partial pressure: and 0.6-0.8Pa, flow: 80sccm, arc current: 80-100A, negative voltage :- 200V, vacuum degree: 4 × 10-3Pa, plated film time: 50-70min.
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.
A kind of high speed steel and preparation method thereof, which is characterized in that it is through the following steps that carry out:
A, it selects common high-speed steel as basis material, machining appropriate is carried out to basis material, is become Meet the tool or mold shape of industrial application standard；Then matrix is carried out carrying out 1240 DEG C of high temperature quenchings and three times 560 The heat treatment of DEG C high tempering, is successively polished with 800#, 1000#, 1500# waterproof abrasive paper on grinding machine, the use of partial size is 0.1 μm diamond be 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 40-45ke V, Ti ion be 45.1, the implantation dosage of 16.5nm, Ti ion is fixed are as follows: 0.6 × 1017-1.0×1017ions/cm2；N ion implanting parameter are as follows: Vacuum chamber background vacuum 1.0x10-3Pa, N20.4-0.6Pa is divided, applies the bias of -2.7~-2.5kV, frequency on matrix For 14-16kHz, the N ion implanting time is 2.0-3.0h；It injects during Ti ion, incident ion and substrate stainless steel surface 90 ° of angles are kept, beam intensity is controlled in 3.7-4.0A/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 certain thickness film as high rigidity surface layer；Wherein, using WH-800 type multi-Arc Ion Plating, coating process ginseng Number is depositing temperature: 430-470 DEG C, nitrogen partial pressure: and 0.6-0.8Pa, flow: 80sccm, arc current: 80-100A, negative voltage :- 200V, vacuum degree: 4 × 10-3Pa, plated film time: 50-70min；
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 certain thickness film as self-lubricating surface layer；Its In, using WH-800 type multi-Arc Ion Plating, coating process parameter is depositing temperature: 430-470 DEG C, nitrogen partial pressure: 0.6- 0.8Pa, flow: 80sccm, arc current: 80-100A, negative voltage: -200V, vacuum degree: 4 × 10-3Pa, plated film time: 50- 70min。
The present invention has the following technical effect that:
(1) present invention provides a kind of high speed steel, and hardness with higher, electric conductivity, is led good machinability It is hot etc.；It is but also with ceramic characteristics, such as higher elasticity modulus, good corrosion resistance and high temperature oxidation resistance simultaneously Deng.
(2) high performance high-speed steel is prepared using this method, condition controllable precise, surface of high speed steel coating functionality are complete Whole, high yield rate solves the secondary lubrication that rubs under the reduction of its hardness elasticity modulus as caused by coating film treatment, different condition The problems such as.Meanwhile also solving the problems, such as that ion is reunited when ion implanting, it is ensured that the uniformity and matrix and film of film Between bond strength.
Detailed description of the invention
Fig. 1 is surface of high speed steel cross-sectional view obtained in the embodiment of the present invention 1.
Fig. 2 is the shape appearance figure of high-speed steel and SiC ball opposite grinding obtained in the embodiment of the present invention 2.
Fig. 3 is the impression figure of high-speed steel binding force test obtained in the embodiment of the present invention 3.
Fig. 4 is the scratch figure of high-speed 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 high speed steel, selection grade of steel are W2Mo9Cr4VCo8, high-speed steel having a size of 60x60mm be matrix material Material, which is characterized in that be followed successively by outward from matrix surface with a thickness of the TiAlN film layer of 80nm and thin with a thickness of the VN of 80nm Film layer.
A kind of preparation method of high speed steel, which is characterized in that it is through the following steps that carry out:
It a, is W to grade of steel2Mo9Cr4VCo8, high speed steel substrate material having a size of 60x60mm carry out it is appropriate mechanical plus Work 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 the heat treatment of 560 DEG C of high temperings three times, it is successively polished, is made with 800#, 1000#, 1500# waterproof abrasive paper on grinding machine Using partial size is that 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 40ke V, Ti ion be 45.1, The implantation dosage of 16.5nm, Ti ion is fixed are as follows: 0.6 × 1017ions/cm2；N ion implanting parameter are as follows: vacuum chamber base vacuum Spend 1.0x10-3Pa, N20.4Pa is divided, the bias of application -2.5kV on matrix, frequency 14kHz, N the ion implanting time is 2.0h；It injects during Ti ion, incident ion and substrate stainless steel surface keep 90 ° of angles, and beam intensity is controlled in 3.7A/ 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 80nm as high rigidity surface layer；Wherein, using WH-800 type multi-Arc Ion Plating, coating process Parameter is depositing temperature: 430 DEG C, nitrogen partial pressure: and 0.6Pa, flow: 80sccm, arc current: 80A, negative voltage: -200V, vacuum degree: 4×10-3Pa, plated film time: 50min；
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 80nm as self-lubricating surface layer； Wherein, using WH-800 type multi-Arc Ion Plating, coating process parameter is depositing temperature: 430 DEG C, nitrogen partial pressure: 0.6Pa, stream Amount: 80sccm, arc current: 80A, negative voltage: -200V, vacuum degree: 4 × 10-3Pa, plated film time: 50min.
Embodiment 2
A kind of high speed steel, selection grade of steel are that selection grade of steel is W6Mo5Cr4V2, high-speed steel having a size of 60x80mm For basis material, which is characterized in that be followed successively by outward from matrix surface with a thickness of 90nm TiAlN film layer and with a thickness of The VN film layer of 90nm.
A kind of preparation method of high speed steel, which is characterized in that it is through the following steps that carry out:
It a, is W to grade of steel6Mo5Cr4V2, high speed steel substrate material having a size of 60x80mm carry out machining appropriate, Become the tool or mold shape for meeting industrial application standard；Then to matrix carry out the quenching of 1240 DEG C of high temperature and The heat treatment of 560 DEG C of high temperings three times is successively polished with 800#, 1000#, 1500# waterproof abrasive paper on grinding machine, uses grain Diameter is that 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 43ke V, Ti ion be 45.1, The implantation dosage of 16.5nm, Ti ion is fixed are as follows: 0.8 × 1017ions/cm2；N ion implanting parameter are as follows: vacuum chamber base vacuum Spend 1.0x10-3Pa, N20.5Pa is divided, the bias of application -2.6kV on matrix, frequency 15kHz, 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 3.8A/ 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 90nm as high rigidity surface layer；Wherein, using WH-800 type multi-Arc Ion Plating, coating process Parameter is depositing temperature: 450 DEG C, nitrogen partial pressure: and 0.7Pa, flow: 80sccm, arc current: 90A, negative voltage: -200V, 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 90nm 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: 0.7Pa, stream Amount: 80sccm, arc current: 90A, negative voltage: -200V, vacuum degree: 4 × 10-3Pa, plated film time: 60min.
Embodiment 3
A kind of high speed steel, selection grade of steel are that selection grade of steel is W18Cr4V, the high-speed steel having a size of 70x70mm is base Body material, which is characterized in that be followed successively by outward from matrix surface with a thickness of the TiAlN film layer of 100nm and with a thickness of 100nm VN film layer.
A kind of preparation method of high speed steel, which is characterized in that it is through the following steps that carry out:
It a, is W to grade of steel is selected18Cr4V, the high speed steel substrate material having a size of 70x70mm carries out machining appropriate, Become the tool or mold shape for meeting industrial application standard；Then to matrix carry out the quenching of 1240 DEG C of high temperature and The heat treatment of 560 DEG C of high temperings three times is successively polished with 800#, 1000#, 1500# waterproof abrasive paper on grinding machine, uses grain Diameter is that 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 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 -2.7kV on matrix, frequency 16kHz, 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 4.0A/ 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 100nm as high rigidity surface layer；Wherein, using WH-800 type multi-Arc Ion Plating, plated film work Skill parameter is depositing temperature: 470 DEG C, nitrogen partial pressure: 0.8Pa, flow: 80sccm, arc current: 100A, 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 100nm as self-lubricating surface layer； Wherein, using WH-800 type multi-Arc Ion Plating, coating process parameter is depositing temperature: 470 DEG C, nitrogen partial pressure: 0.8Pa, stream Amount: 80sccm, arc current: 100A, negative voltage: -200V, vacuum degree: 4 × 10-3Pa, plated film time: 70min.
High-speed 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 high-speed 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 5N, angle of rotation Speed is 95.49rmp, abrasion radius is 3.00mm, 100,000 turns of abrasion；Surface of high speed steel after experiment is without significant change, aobvious Micro- 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 hard It spends anti abrasive high-speed steel and 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 high speed steel, selection high-speed steel is basis material, it is characterised in that: is followed successively by outward from matrix surface TiAlN film layer and VN film layer；The TiAlN thin film layer thickness is 80nm-100nm, and the VN thin film layer thickness is 80nm-100nm。
2. a kind of preparation method of high speed steel according to claim 1, selection regular high speed steels are basis material, It is characterized in that, it is through the following steps that carry out: matrix being machined first, is heat-treated, is polished and polishing treatment, Then it cleaned, dried, the ion implanting of titanium and nitrogen dual element is carried out using ion implantation, then in multi-arc ion plating film Depositing Ti AlN film layer in machine, then VN film layer is deposited in multi-Arc Ion Plating.
3. a kind of preparation method of high speed steel according to claim 2, it is characterised in that: the ion implantation Ti The energy of ion are as follows: the projected range Rp and range straggling of 40-45keV, Ti ion are 45.1,16.5nm, the injection of Ti ion Dosage is fixed are as follows: 0.6 × 1017-1.0×1017ions/cm2；N ion implanting parameter are as follows: vacuum chamber background vacuum 1.0x10- 3Pa, N20.4-0.6Pa is divided, applies the bias of -2.7~-2.5kV on matrix, when frequency 14-16kHz, N ion implanting Between be 2.0-3.0h；It injects during Ti ion, incident ion and substrate stainless steel surface keep 90 ° of angles, beam intensity control System is in 3.7-4.0A/cm2, effect is increased to avoid temperature caused by ion implantation process；It injects during N ion, N ion hangs down It is straight incident.
4. a kind of preparation method of high speed steel according to claim 3, it is characterised in that: the multi-arc ion plating film Machine uses WH-800 type multi-Arc Ion Plating, and main coating process parameter is depositing temperature: 430-470 DEG C, nitrogen partial pressure: 0.6-0.8Pa, flow: 80sccm, arc current: 80-100A, negative voltage: -200V, vacuum degree: 4 × 10-3Pa, plated film time: 50-70min。
5. a kind of preparation method of high speed steel according to claim 4, it is characterised in that: described in multi-arc ion coating Depositing Ti AlN film layer is using high purity titanium and rafifinal as target in film machine, and is passed through nitrogen；It sinks in multi-Arc Ion Plating Product VN film layer is passed through nitrogen using high purity vanadium as target.
CN201910627657.3A 2019-07-12 2019-07-12 A kind of high speed steel and preparation method thereof Withdrawn CN110373637A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110863182A (en) * 2019-11-12 2020-03-06 东风商用车有限公司 Method for strengthening surface coating of gear cold extrusion die

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2010115760A (en) * 2008-11-14 2010-05-27 Sumitomo Electric Hardmetal Corp Surface-coated cutting tool
CN108179375A (en) * 2018-01-30 2018-06-19 哈尔滨工程大学 The carburizing of alloy steel products surface vacuum and ion implanting compound hardening treatment method

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2010115760A (en) * 2008-11-14 2010-05-27 Sumitomo Electric Hardmetal Corp Surface-coated cutting tool
CN108179375A (en) * 2018-01-30 2018-06-19 哈尔滨工程大学 The carburizing of alloy steel products surface vacuum and ion implanting compound hardening treatment method

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110863182A (en) * 2019-11-12 2020-03-06 东风商用车有限公司 Method for strengthening surface coating of gear cold extrusion die

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Application publication date: 20191025