CN108070817A - A kind of compound dual treatment method of metal die steel surface - Google Patents

A kind of compound dual treatment method of metal die steel surface Download PDF

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CN108070817A
CN108070817A CN201611011000.7A CN201611011000A CN108070817A CN 108070817 A CN108070817 A CN 108070817A CN 201611011000 A CN201611011000 A CN 201611011000A CN 108070817 A CN108070817 A CN 108070817A
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steel surface
ion
metal die
mold
die steel
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CN108070817B (en
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彭继华
苏东艺
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GUANGZHOU GRANDTECH CO Ltd
South China University of Technology SCUT
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GUANGZHOU GRANDTECH CO Ltd
South China University of Technology SCUT
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    • 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
    • C23C8/00—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals
    • C23C8/02—Pretreatment of the material to be coated
    • 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
    • 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
    • C23C8/00—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals
    • C23C8/06—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using gases
    • C23C8/36—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using gases using ionised gases, e.g. ionitriding
    • C23C8/38—Treatment of ferrous surfaces

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Physical Vapour Deposition (AREA)

Abstract

The present invention provides a kind of compound dual treatment method of metal die steel surface, including：The cleaning of metal die steel surface, metal die steel surface drying pretreatment implement ion etching, using assisting ion source using assisting ion source to the indoor mold steel surface of vacuum, mold is realized after carbon Nitrogen ion permeation, carbon Nitrogen ion permeation and argon ion bombardment etching surface to be implemented using assisting ion source again and mold is applied to using asymmetric bipolar pulsed bias pattern, cathodic arc discharge method coating PVD coatings and etc..This metal mould steel surface recombination dual treatment method can realize die surface all standing, the reinforcing without dead angle, simultaneously PVD coatings are coated using cathodic arc discharge method, enhance groove and blind hole by frequency, the reasonable change of duty cycle to adsorb the reception of deposited particles, blind hole on mold, the PVD coatings of narrow slot surface acquisition thickness as far as possible are further improved, so as to prepare the coating of antioxidant height, excellent in abrasion resistance in die surface.

Description

A kind of compound dual treatment method of metal die steel surface
Technical field
The present invention relates to Treatment of Metal Surface, and in particular to mould steel Surface hardening treatment and by physical vapour deposition (PVD) from And obtain high-bond, the composite treatment technology of wear-and corrosion-resistant film coating.
Background technology
Metal base mold is the important tool of modern advanced manufacturing industry large-scale production.From operating temperature when using Division, has mold heat, cold mold, plastic mould, the mold base material of selection is respectively hot die steel, cold work die steel；From adding Work shape angles divide, and have casting mould, mold for extruding and forming etc..Because the working condition of mold, filled except mold is required to have Outside the obdurability of foot, surface high-wearing feature, anti-caking, resistance to marring, fatigue resistance are also required.Therefore current universal means It is the requirement for meeting high-wearing feature, anti-caking, resistance to marring, fatigue resistance using process for treating surface.According to different Applying working condition, a variety of process for treating surface of die industry development and application at present, such as plating/chemical plating, Surface heat-treatent (such as sensing heating, laser treatment), surface metal diffusion penetration (such as Mo, V), the nonmetallic diffusion penetration in surface (molten C, N, O, S, Si, B etc.), surface vapor is deposited (including physical vapour deposition (PVD) (PVD) and chemical vapor deposition (CVD)) etc..In view of mould The performance of tool steel in itself varies with temperature and the stability requirement of die size, and many needs are when longer more than 600 DEG C or more Between the above-mentioned technology implemented be not appropriate for surface treatment applied to high-accuracy mold, otherwise will bring it is complicated it is quenched, adjust ruler The postprocessing working procedures such as very little, reconditioning.
When die surface is nitrogenized using single ionic, for treatment temperature often at 500-600 DEG C, processing time is long, usually exists Nitridation layer surface forms compound layer and (is commonly called as " nitride layer, white layer ") (such as Chinese patent CN104178771A), causes sub-surface region Alloying element dilution.Nitride layer, white layer easily becomes the destruction source of nitration coating layer during use.Using C-N permeation (such as Chinese patents CN104152916A) although can effectively inhibit the nitride layer, white layer of layer surface, the hardness not more than HV 1300 of infiltration layer, And red hardness is poor, limits further improving for die life.Chinese patent CN101058870A die surfaces are using single The combination power of PVD coatings, coating and matrix is weak and PVD coatings with the mechanical matching difference of matrix are limitation PVD coating high rigidity And the lethal factor that the advantages such as low-friction coefficient play.Example is reported directly in mould in disclosed patent CN103286919A recently Benevolence surface prepares graphene film using high temperature and pressure CVD method, reports undeclared mode base material, but infers that this method is not suitable for answering For steel-based mold, because the base material that CVD surfaces can grow graphene so far is also mainly the metals such as Cu/Ni/Ir/Au.In State patent CN102105243A is also a kind of CVD method, be substantially formed on die casting surface C-S co-penetration layers-containing nanotube/ Then the carbon film of silk covers traditional releasing agent in coating surface in surface smear fullerene powder, use, can improve mold and resist Viscous aluminium ability.
In general, the coating surface hardness that physical gas-phase deposite method (PVD) obtains can reach more than HV2000, even Obtain superhard coating；Preparation technology of coating temperature control is less than 500 DEG C, and therefore, PVD coatings have high wear-resisting, tension Hinder performance, meet requirement of the metal die to surface abrasion resistance；And PVD preparation process will not cause matrix to change substantially, The size of mold is unaffected.Therefore, PVD technique is in die surface process field great potential.But directly in mould steel table Face prepares PVD coatings, because matrix hardness, elasticity modulus, coefficient of thermal expansion etc. and PVD coatings have larger difference, it is difficult to obtain The PVD coatings of high-bond, PVD coatings easily fail during use.On the other hand, the mold of complex geometry is often deposited In the big blind hole of aspect ratio value or deep and narrow groove, it is difficult to only with PVD technique obtain uniform painting in these regions Layer in addition there are uncoated regions.Even if PVD coatings can give full play to its advantage, the failure of mold is also easily from blind hole, narrow Start at slot.In recent years, although there are reports both at home and abroad is related to the molds of mold steel surface or some simple surface shapes After (such as die casting pin) uses ionic nitriding, surface polishing removal nitride layer, white layer, then the technology of PVD processing is carried out, but ion It with reference to matching difference is still the main problem faced to nitrogenize between the nitride layer, white layer and PVD layer generated, for elimination nitride layer, white layer PVD is caused to apply Layer combines this weak problem of power, and sandblasting is polished after ionic nitriding and removes the nitride layer, white layer.Nitride layer, white layer in simple surface easily removes, Above-mentioned mold medium-length hole, narrow slot position are then not easy, and the nitride layer, white layer that these positions are difficult to eliminate is likely to become in mold usage Weak link.No matter simply this requires the surface treatment of mold that should meet claimed below, the surface region of one side mold work, Plane, curved surface, surface of deep hole, narrow slot surface obtain fully reinforcing after being required to surface treatment；On the other hand, the table of acquisition is handled Surface layer between matrix have high bond strength, and coating have high rigidity, high red hardness and high antioxidant, high thermal fatigue resistance Property.
The content of the invention
In view of the deficiencies of the prior art, the technical problems to be solved by the invention are, for mould steel feature and mold The characteristics of complex-shaped, proposition is a kind of can be realized die surface all standing, the reinforcing without dead angle and effectively realize film base junction Close efficient cryogenic ion carbonitriding and the compound die surface processing side of physical vapour deposition (PVD) of intensity height, excellent in abrasion resistance Method.
To realize above-mentioned technical proposal, the present invention provides a kind of compound dual treatment method of metal die steel surface, tools Body comprises the following steps：
1) metal die steel surface cleans：Mould steel surface and oil contaminant is removed using commercial metals cleaning agent, after rinsing drying For use；
2) metal die steel surface drying pretreatment：The mould steel rinsed after drying is fixed on to the workpiece of Hauzer devices On frame, door for vacuum chamber is closed, and starts work rest rotation, vacuum chamber is extracted into vacuum less than 5x10-3Pa opens auxiliary heating dress It puts, the vacuum chamber containing mould steel is warming up to 300-400 DEG C；
3) ion etching is implemented to the indoor mold steel surface of vacuum using assisting ion source：Using heated filament DC arc ion The ar-ion beam that source obtains, is passed through argon gas, and pressure in vacuum tank is made to apply for 0.1Pa, beam current 70-100A to mould steel 200V is biased, using Dc bias pattern, argon ion bombardment etched mold steel surface 30-90 minutes；
4) using assisting ion source, carbon Nitrogen ion permeation is realized to mold：Vacuum indoor temperature is kept to maintain 300-400 DEG C, and the argon flow amount and ion beam current of heated filament DC arc ion source in step 3) are maintained, it is passed through nitrogen, first in vacuum chamber After vacuum chamber vacuum reaches 2.0-5.0Pa, it is straight for 400-600V to adjust workpiece Dc bias for the hybrid working gas of alkane, hydrogen Glow discharge occurs for stream, mold steel surface, keeps the infiltration layer rate of carbo-nitriding as micro- m/h of 40-60, infiltration layer as needed Thickness controls the carbo-nitriding time, after ion permeation, closes hybrid working gas, and it is 150V to adjust mold Dc bias, Argon ion bombardment die surface closes ion source after 15-30 minutes；
5) argon ion bombardment etching surface is implemented using assisting ion source again after the permeation of carbon Nitrogen ion；
6) mold, cathodic arc discharge method coating PVD coatings are applied to using asymmetric bipolar pulsed bias pattern.
Preferably, cathodic arc discharge method prepares PVD coatings and is as follows in the step 6)：
61) nitrogen is passed through into vacuum chamber, pressure in vacuum tank is made to remain 0.5-1Pa；
62) asymmetric bipolar pulsed bias pattern, frequency 300-30kHz are opened, negative pulse peak value is 50-150V, just Peak value of pulse is 10-20V, duty cycle 30-80%；
63) pure metalic cathode electric arc target is opened, target current 100-120A prepares 0.5-1.0 microns thick binary nitride layer Metallic cathode electric arc target is closed afterwards；
64) the alloy cathode electric arc target of rich aluminium is opened, target current 100-120A prepares 3-4 microns thick multicomponent nitride layer After close alloys target；
65) after vacuum room temperature is cooled to less than 100 DEG C, door for vacuum chamber is opened, takes out workpiece.
In the above-mentioned technical solutions, the device that in the present invention prepared by PVD coatings is routine techniques, using Dutch HAUZER Flexicoat-850 vacuum coaters (hereinafter referred to as HAUZER devices).This metal mould steel surface recombination Duplex treatment side Method is aided in by high density ion source, and die surface low-temperature ion carbo-nitriding is realized at a temperature of less than 400 DEG C, obtains 30- 50 micron thickness infiltration layers so that die surface hardness is more than HV1000；Carbo-nitriding simultaneously avoids nitride layer, white layer from occurring, and infiltration layer Hardness, elasticity modulus are reduced from surface to core matrix in slow gradient, and solving existing report, there are nitride layer, white layers to lead because of nitration case The problem of causing PVD coating binding forces poor；PVD coatings are coated using cathodic arc discharge method, pass through the reasonable change of frequency, duty cycle Change enhancing groove and blind hole to adsorb the reception of deposited particles, further improve blind hole on mold, narrow slot surface obtains as far as possible Thick PVD coatings；So as to prepare the coating of antioxidant height, excellent in abrasion resistance in die surface.
Preferably, the permeation of carbon Nitrogen ion uses nitrogen, methane, the hybrid working gas of hydrogen in the step 4), wherein The percent by volume of methane gas is 10-25%, and the percent by volume of hydrogen is 40-60%, remaining as nitrogen.
Preferably, the 15-30 minutes argon ion etching time in the step 5) after carbon Nitrogen ion permeation, beam current 70- 100A。
Preferably, the PVD coatings prepared in the step 6) are the composite coatings of binary nitride and multicomponent nitride.
Preferably, the binary nitride is one kind in TiN or CrN.
Preferably, the multicomponent nitride is the Al-Me-N nitride rich in aluminium, and wherein Me is at least in Cr, Ti One kind can include V, Si, Nb, one kind in Y.
The present invention is compared with the advantageous effect of the prior art：
(1) present invention realizes complicated shape mold work region all standing and strengthens, solution be using high density from Component aids in, and die surface low-temperature ion carbo-nitriding is realized at a temperature of less than 400 DEG C, obtains 30-50 micron thickness infiltration layers, So that die surface hardness is more than HV1000；Plasma asistance carbo-nitriding can cover the areas such as face and the narrow slot of complicated shape Domain.
(2) present invention solves the problems, such as existing report there are nitride layer, white layers to cause PVD coating binding forces poor because of nitration case, solution Scheme is using rational carbo-nitriding nitride layer, white layer to be avoided to occur, and the hardness of infiltration layer, elasticity modulus are from surface to core matrix It is reduced in slow gradient.
(3) present invention is to further improve blind hole on mold, the PVD coatings of narrow slot surface acquisition thickness as far as possible, solution party Case is to apply bipolar pulse bias in workpiece surface when preparing PVD coatings, enhances groove by frequency, the reasonable change of duty cycle The reception of deposited particles is adsorbed with blind hole, from the coating that antioxidant height, excellent in abrasion resistance are prepared in die surface.
Description of the drawings
Fig. 1 is process method step schematic diagram in the present invention.
Specific embodiment
To more fully understand the present invention, the present invention is described in detail with reference to the accompanying drawings and examples, but the present invention Embodiment it is unlimited so.
Embodiment 1
A kind of compound dual treatment method of metal die steel surface with reference to shown in Fig. 1, specifically includes following steps：
1) choose the polishing of H13 steel and sandblasting test piece (processing of quenched and double annealing, hardness HRC50) is inserted containing 5wt% In the aqueous solution of commercially available " strong " metal degreasing dirt cleaning agent, boil about after five minutes, by test piece with deionized water rinsed clean simultaneously In the deionized water solution of the 1063 reagent 100mL/L containing German bohr company antirust, impregnate 10 seconds, oil free compression is used after taking-up Air blow drying, when 80 DEG C of drying 1 are small after it is for use；Test piece dress is hung over, HAUZER devices are put on fixture；
2) door for vacuum chamber is closed, and starts work rest rotation；Vacuum chamber is pumped to back end vacuum 5x10-3Auxiliary is opened after Pa Vacuum chamber is warming up to 300 DEG C by heating unit；
3) argon gas is passed through, it is 0.1Pa, beam current 70A to make pressure in vacuum tank；Workpiece is biased 200V, using straight Flow bias mode；Argon ion bombardment etched mold surface 30 minutes；
4) argon flow amount and ion beam current of heated filament DC arc ion source in step 3) are maintained；Nitrogen is passed through in vacuum chamber Gas, methane, the hybrid working gas of hydrogen, the wherein percent by volume of methane gas are 10%, and the percent by volume of hydrogen is 40%, remaining is nitrogen；After vacuum chamber vacuum reaches 2.0Pa, it is 400V direct currents to adjust workpiece Dc bias, and brightness occurs for die surface Light discharges；After (obtaining 45 microns of alloying layer thickness) when controlling carbo-nitriding 1 small, hybrid working gas is closed, adjusts mold direct current It biases as 150V, argon ion bombardment die surface closes ion source after 15 minutes；
5) nitrogen is passed through in vacuum chamber, pressure in vacuum tank is made to remain 0.5Pa；Open asymmetric bipolar pulsed bias mould Formula, frequency 300Hz, negative pulse peak value be 150V, positive pulse peak value be 20V, duty cycle 30%；Open cathode arc Cr Target, target current 100A close electric arc target after preparing 0.5 micron of thickness CrN；Open Al70Cr30Alloy cathode electric arc target, target current 100A prepares 3 microns of thickness Al70Cr30Alloys target is closed after N layers.After vacuum room temperature is cooled to 100 DEG C, door for vacuum chamber is opened, Take out workpiece.
Visually observation, coating uniform are fine and close.Coating and basal body binding force HF1 after rockwell indentation evaluation processing.
The H13 steel surfaces region obtained after above-mentioned processing, no matter simple flat surface, curved surface, surface of deep hole, narrow slot surface Obtain abundant reinforcing；Meanwhile the PVD coatings for handling acquisition pass through with the bond strength between H13 steel matrix with height PVD coatings improve hardness, red hardness, inoxidizability and the thermal fatigue resistance of H13 steel.
Embodiment 2
A kind of compound dual treatment method of metal die steel surface with reference to shown in Fig. 1, specifically includes following steps：
1) choose the polishing of M35 steel and sandblasting test piece (processing of quenched and double annealing, hardness HRC62) is inserted containing 5wt% In the aqueous solution of commercially available " strong " metal degreasing dirt cleaning agent, boil about after five minutes, by test piece with deionized water rinsed clean simultaneously In the deionized water solution of the 1063 reagent 100mL/L containing German bohr company antirust, impregnate 5 seconds, oil free compression is used after taking-up Air blow drying, when 80 DEG C of drying 1 are small after it is for use；Test piece dress is hung over, HAUZER devices are put on fixture；
2) door for vacuum chamber is closed, and starts work rest rotation；Vacuum chamber is pumped to back end vacuum 7x10-3Auxiliary is opened after Pa Vacuum chamber is warming up to 400 DEG C by heating unit；
3) argon gas is passed through, it is 0.1Pa, beam current 100A to make pressure in vacuum tank；Workpiece is biased 200V, using straight Flow bias mode；Argon ion bombardment etched mold surface 60 minutes；
4) argon flow amount and ion beam current of heated filament DC arc ion source in step 3) are maintained；Nitrogen is passed through in vacuum chamber Gas, methane, the hybrid working gas of hydrogen, the wherein percent by volume of methane gas are 25%, and the percent by volume of hydrogen is 55%, remaining is nitrogen；After vacuum chamber vacuum reaches 5.0Pa, it is 600V direct currents to adjust workpiece Dc bias, and brightness occurs for die surface Light discharges；After controlling carbo-nitriding 40 minutes (obtaining 60 microns of alloying layer thickness), hybrid working gas is closed, adjusts mold direct current It biases as 150V, argon ion bombardment die surface closes ion source after twenty minutes；
5) nitrogen is passed through in vacuum chamber, pressure in vacuum tank is made to remain 1Pa；Asymmetric bipolar pulsed bias pattern is opened, Frequency is 30kHz, and negative pulse peak value is 50V, and positive pulse peak value is 10V, duty cycle 80%；Open cathode arc Ti targets, target Electric current 120A closes electric arc target after preparing 1 micron of thickness TiN；Open Al65Cr35It is prepared by alloy cathode electric arc target, target current 100A 4 microns of thickness Al65Cr35Alloys target is closed after N layers.After vacuum room temperature is cooled to 100 DEG C, door for vacuum chamber is opened, takes out workpiece.
Visually observation, coating uniform are fine and close.Coating and basal body binding force HF1 after rockwell indentation evaluation processing.
The M35 steel surfaces region obtained after above-mentioned processing, no matter simple flat surface, curved surface, surface of deep hole, narrow slot surface Obtain abundant reinforcing；Meanwhile the PVD coatings for handling acquisition pass through with the bond strength between M35 steel matrix with height PVD coatings improve hardness, red hardness, inoxidizability and the thermal fatigue resistance of H13 steel.
Embodiment 3
A kind of compound dual treatment method of metal die steel surface with reference to shown in Fig. 1, specifically includes following steps：
1) 1 set of phone housing part extrusion die, manufactured by H13 (quenched and double annealing is handled, hardness HRC50) and The automatic Cleaning Line cleaning of Jin Tai companies is inserted in the H13 mould steel polishing test piece of same hardness, by the workpiece deionization after cleaning Water rinsed clean and in the deionized water solution of the 1063 reagent 100mL/L containing German bohr company antirust impregnates 15 seconds, takes out Dried up afterwards with oil-free compressed air, when 80 DEG C of drying 1 are small after it is for use；Workpiece dress is hung over, HAUZER devices are put on fixture；
2) door for vacuum chamber is closed, and starts work rest rotation；Vacuum chamber is pumped to back end vacuum 5x10-3Auxiliary is opened after Pa Vacuum chamber is warming up to 400 DEG C by heating unit；
3) argon gas is passed through, it is 0.1Pa, beam current 90A to make pressure in vacuum tank；Workpiece is biased 200V, using straight Flow bias mode；Argon ion bombardment etched mold surface 90 minutes；
4) argon flow amount and ion beam current of heated filament DC arc ion source in step 3) are maintained；Nitrogen is passed through in vacuum chamber Gas, methane, the hybrid working gas of hydrogen, the wherein percent by volume of methane gas are 15%, and the percent by volume of hydrogen is 45%, remaining is nitrogen；After vacuum chamber vacuum reaches 3.5Pa, it is 500V direct currents to adjust workpiece Dc bias, and brightness occurs for die surface Light discharges；After controlling carbo-nitriding 30 minutes (obtaining 43 microns of alloying layer thickness), hybrid working gas is closed, adjusts mold direct current It biases as 150V, argon ion bombardment die surface closes ion source after 30 minutes；
5) nitrogen is passed through in vacuum chamber, pressure in vacuum tank is made to remain 0.6Pa；Open asymmetric bipolar pulsed bias mould Formula, frequency 10kHz, negative pulse peak value be 80V, positive pulse peak value be 15V, duty cycle 50%；Cathode arc Cr targets are opened, Target current 120A closes electric arc target after preparing 1 micron of thickness CrN；Open Al65Cr35Alloy cathode electric arc target, target current 100A, system Standby 3.5 microns of thickness Al65Cr35Alloys target is closed after N layers.After vacuum room temperature is cooled to 70 DEG C, door for vacuum chamber is opened, takes out work Part.
Visually observation, coating uniform are fine and close.Coating and basal body binding force HF1 after rockwell indentation evaluation processing.
The above is presently preferred embodiments of the present invention, but the present invention should not be limited to the embodiment and attached drawing institute is public The content opened so every do not depart from the lower equivalent or modification completed of spirit disclosed in this invention, both falls within protection of the present invention Scope.

Claims (10)

1. a kind of compound dual treatment method of metal die steel surface, it is characterised in that comprise the following steps：
1) metal die steel surface cleans；
2) metal die steel surface drying pretreatment；
3) ion etching is implemented to the indoor mold steel surface of vacuum using assisting ion source；
4) using assisting ion source, carbon Nitrogen ion permeation is realized to mold；
5) argon ion bombardment etching surface is implemented using assisting ion source again after the permeation of carbon Nitrogen ion；
6) mold, cathodic arc discharge method coating PVD coatings are applied to using asymmetric bipolar pulsed bias pattern.
2. the compound dual treatment method of metal die steel surface as described in claim 1, it is characterised in that：In the step 2) Metal die steel surface drying pretreatment method is specially that the mould steel rinsed after drying is fixed on work rest, closes vacuum Room door, and work rest rotation is started, vacuum chamber is extracted into vacuum less than 5x10-3Pa opens assisted heating device, will contain mold The vacuum chamber of steel is warming up to 300-400 DEG C.
3. the compound dual treatment method of metal die steel surface as described in claim 1, it is characterised in that：In the step 3) The method of ion etching is specially the ar-ion beam obtained using heated filament DC arc ion source, is passed through argon gas, makes pressure in vacuum tank 200V is biased to mould steel for 0.1Pa, beam current 70-100A, using Dc bias pattern, argon ion bombardment is carved Lose mold steel surface 30-90 minutes.
4. the compound dual treatment method of metal die steel surface as described in claim 1, it is characterised in that：In the step 4) The specific method of carbon Nitrogen ion permeation is that vacuum indoor temperature is kept to maintain 300-400 DEG C, and maintains heated filament in step 3) straight The argon flow amount and ion beam current of arc ion source are flowed, the hybrid working gas of nitrogen, methane, hydrogen is passed through in vacuum chamber, very After empty room vacuum reaches 2.0-5.0Pa, it is 400-600V direct currents to adjust workpiece Dc bias, and mold steel surface occurs aura and puts Electricity keeps the infiltration layer rate of carbo-nitriding as micro- m/h of 40-60, and alloying layer thickness as needed controls the carbo-nitriding time, After ion permeation, hybrid working gas is closed, it is 150V, argon ion bombardment die surface 15- to adjust mold Dc bias Ion source is closed after 30 minutes
5. the compound dual treatment method of metal die steel surface as described in claim 1, it is characterised in that：In the step 6) Cathodic arc discharge method prepares PVD coatings and is as follows,
61) nitrogen is passed through into vacuum chamber, pressure in vacuum tank is made to remain 0.5-1Pa；
62) asymmetric bipolar pulsed bias pattern, frequency 300-30kHz are opened, negative pulse peak value is 50-150V, positive pulse Peak value is 10-20V, duty cycle 30-80%；
63) pure metalic cathode electric arc target is opened, target current 100-120A is closed after preparing 0.5-1.0 microns thick binary nitride layer Close metallic cathode electric arc target；
64) the alloy cathode electric arc target of rich aluminium is opened, target current 100-120A is closed after preparing 3-4 microns thick multicomponent nitride layer It is closed gold target；
65) after vacuum room temperature is cooled to less than 100 DEG C, door for vacuum chamber is opened, takes out workpiece.
6. the compound dual treatment method of metal die steel surface as claimed in claim 4, it is characterised in that：In the step 4) The permeation of carbon Nitrogen ion is 10- using nitrogen, methane, the hybrid working gas of hydrogen, the wherein percent by volume of methane gas 25%, the percent by volume of hydrogen is 40-60%, remaining as nitrogen.
7. the compound dual treatment method of metal die steel surface as described in claim 1, it is characterised in that：In the step 5) 15-30 minutes argon ion etching time after carbon Nitrogen ion permeation, beam current 70-100A.
8. the compound dual treatment method of metal die steel surface as described in claim 1, it is characterised in that：In the step 6) The PVD coatings of preparation are the composite coatings of binary nitride and multicomponent nitride.
9. the compound dual treatment method of metal die steel surface as claimed in claim 8, it is characterised in that：The binary nitridation Object is one kind in TiN or CrN.
10. the compound dual treatment method of metal die steel surface as claimed in claim 8, it is characterised in that：Described is polynary Nitride is the Al-Me-N nitride rich in aluminium, and wherein Me is at least one kind in Cr, Ti, can include V, Si, Nb, one in Y Kind.
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CN110343993A (en) * 2019-08-07 2019-10-18 广东工业大学 A kind of carbide surface processing method and application
CN113249680A (en) * 2021-05-13 2021-08-13 江苏新合益机械有限公司 Surface treatment method of high-strength corrosion-resistant precision piston rod

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CN105132876A (en) * 2015-09-15 2015-12-09 辽宁科技大学 Surface compound treatment method for steel gear
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CN108893707A (en) * 2018-07-23 2018-11-27 江苏苏德涂层有限公司 Aluminium die casting surface coated treatment technique and the cated aluminium die casting of tool
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