CN109023285B - A kind of Ti (C, N)/Cr (C, N) complex gradient wear-resistant alloy layer and preparation method thereof - Google Patents

A kind of Ti (C, N)/Cr (C, N) complex gradient wear-resistant alloy layer and preparation method thereof Download PDF

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CN109023285B
CN109023285B CN201811055651.5A CN201811055651A CN109023285B CN 109023285 B CN109023285 B CN 109023285B CN 201811055651 A CN201811055651 A CN 201811055651A CN 109023285 B CN109023285 B CN 109023285B
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layer
gear
wear
valve
opened
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CN109023285A (en
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魏东博
张平则
梁宏璇
刘子利
李淑琴
姚正军
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Nanjing University of Aeronautics and Astronautics
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    • 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
    • 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
    • C23C14/022Cleaning or etching treatments by means of bombardment with energetic particles or radiation
    • 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
    • C23C14/0664Carbonitrides
    • 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
    • C23C14/14Metallic material, boron or silicon
    • C23C14/18Metallic material, boron or silicon on other inorganic substrates
    • 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
    • C23C14/34Sputtering
    • C23C14/46Sputtering by ion beam produced by an external ion source

Abstract

The invention discloses a kind of Ti (C, N)/Cr (C, N) complex gradient wear-resistant alloy layer and preparation method thereof, which successively includes Ti-Cr sedimentary, Ti (C, N)/Cr (C, N) graded ceramics layer and C, N strengthening layer from top to bottom.Preparation method is the following steps are included: (1) injects C, N strengthening layer in powder metallurgical gear surface ion;(2) strengthen the double brightness plasma alloying methods of layer surface in C, N and prepare Ti-Cr alloy-layer.C, N atom easily interacts with alloying element, generates nitride, carbide.During plasma alloying, C, N of Ti, Cr and ion implanting for sputtering react, and form with Ti (C, N)/Cr (C, N) composite construction graded ceramics wear-resistant alloy layer.The wear-resisting property of powder metallurgical gear is greatly improved in the present invention, substantially extends the service life of gear.

Description

A kind of Ti (C, N)/Cr (C, N) complex gradient wear-resistant alloy layer and preparation method thereof
Technical field
The invention belongs to material science and technology field, in particular to a kind of powder metallurgy toothed wheel surface Ti (C, N)/Cr (C, N) the graded ceramics wear-resistant alloy layer and its preparation process of composite construction.
Background technique
For gear, powder metallurgy can reduce cast component segregation and heat-treatment processing process time length, energy consumption Big problem makes gear have superior overall performance and economic performance, can effectively lower the manufacturing cost of gear.But tooth Wheel stress condition in transmission is more complicated, and forms of motion is also varied, therefore the form of gear destruction also has multiplicity Change.All in all, gear destruction mainly has broken teeth, destructive glued and destructive pitting these three forms.In order to extend gear Service life makes gear be able to bear the damage of diversified forms, this just needs to improve the wear-resisting property of powder metallurgy toothed wheel surface.
According to current research, there are mainly two types of the modes for improving powder metallurgical gear wear-resisting property, first is that Integral alloy, The alloy of invigoration effect using to(for) driven gears.Conventional machining process generallys use this mode, but Integral alloy chemical industry skill It is at high cost, it pollutes larger;Second is that improving gear wear-resisting property by advanced process for modifying surface, formed on driven gears surface Modified layer improves the friction and wear behavior of gear.Abrasion is usually to be modified since material surface, therefore through surface to improve The wear-resisting property of gear is a kind of more common method.These process for modifying surface mainly include that carburizing, nitriding, carbon nitrogen are total Infiltration, thermal spraying, ion implanting, vacuum ion plating etc..The coating and gear prepared using hot-spraying technique is in mechanical bond, in conjunction with The problems such as intensity is low, is easy to appear hole, micro-crack, disbonding in use, reduces the combination of coating and gear Intensity;The ion that ion implantation technology can will improve the element of wear-resisting property injects in gear in vacuum system, to be formed The implanted layer that wear-resisting property is improved.But ion implanted layer thickness is not high, and can only carry out straight line injection, cannot improve comprehensively The wear-resisting property of gear;The surface alloying layer of double brightness plasma alloying technology preparations includes alloy-layer and diffusion layer, ingredient, property It can be distributed with concentration gradient, be firmly combined with matrix, and alloy-layer dense structure, the defects of tight, crackle, working efficiency It is high.
Double-deck glow plasma surface metallurgical technology (hereinafter referred to as " two-lime piles "), is Chinese scholar in ionic nitriding On the basis of independent invention the new Alloying on Metal Planes technology of one kind.Working principle is in a vacuum tank, and furnace body is made For plus earth, two cathodes are respectively set, a placement workpiece is placed for one and provides the source electrode of alloying element, is passed through certain The argon gas of air pressure.Two sets of independent power supplys are set in furnace, and anode and source electrode and anode and workpiece interpolar are distinguished after on-load voltage Aura is generated, i.e., " double-deck glow ".Argon ion bombardment target, it is extremely first to sputter target caused by glow discharge on source electrode Element;And the sputtering of workpiece pole can then heat workpiece.Source voltage is set to be lower than workpiece current potential, while making source power density Higher than workpiece power density.In this way, source electrode sputtering amount will be much larger than the reverse sputtering amount of cathode.At high temperature, the alloy in target Element is deposited and is diffused in workpiece surface formation alloy-layer.Alloy-layer is by alloying element to spreading simultaneously inside basis material It is formed with matrix element interaction.
" coal mine machinery " volume 28 the 7th published in 2007 is interim, and " austenitic stainless steel C, N are ion-implanted surface-modified The side for improving hardness and wear-resisting property in the injection of austenite stainless steel surface C, N using ion implanting is disclosed herein in research " one Method;" vacuum science and the Technology " published volume 30 the 3rd interim " ion implanting space gear driving pair use in 2010 30CrMnSi material vacuum tribological Properties " one are disclosed herein injects Ti, C, N member using ion implanting on gear Element, the method for improving gear wear-resisting property.But the shortcomings that ion implantation technique is that injection layer depth is insufficient, and thickness is small, this is also limited Its application on gear surface reinforcement technique is made;" Materials Science and Engineering journal " the 3rd phase of volume 26 published in 2008 In " influence of double brightness C, N, Ti infiltrations sequence to diffusion layer organization and performance " one be disclosed herein using two-lime piles in 20 steel tables Face carries out the ternary co-osmosized method of C, N, Ti;" metal heat treatmet " interim " Ti6Al4V alloy of volume 37 the 1st published in 2012 The frictional behaviour of surface Ti (C, N) modified layer " one, which is disclosed herein, carries out C, N permeation on the surface Ti6Al4V using double brightness to mention The method of high-wear resistance.
Since powder metallurgical gear wear-resisting property is not able to satisfy requirement, it is wear-resisting to improve its to need process for modifying surface Performance.But presently disclosed research is using a kind of wear-resisting property of surface modifying method raising matrix, and existing modification mostly There are respective problems for technology, such as: single ion implantation, implanted layer is thin, and wearability promotion is limited, thus leads to implanted layer Service life under operating condition is shorter;But simple double brightness plasma alloying temperature are higher, gear shifting quadrant texturing are likely to result in, to its group Knitting structure influences, and declines the overall performance of gear.
In order to meet the requirement of gear high-wear resistance, need to be used in combination using two or more modification modes.But it is single There are limitation, advantage is difficult to realize maximize one technology.Injection depth such as ion implanting is insufficient, and implanted layer is thin, to tooth The wearability promotion of wheel is limited, causes implanted layer service life under working condition shorter;Double brightness plasma alloying technologies can be Gear surface prepares certain thickness alloy-layer, though the metallurgical bonding with matrix may be implemented, simple double brightness plasmas Alloying temperature is higher, is likely to result in gear shifting quadrant texturing, influences on its institutional framework, declines the overall performance of gear.
Summary of the invention
In view of the above problems, the object of the present invention is to provide a kind of Ti (C, N)/Cr (C, N) complex gradient wear-resistant alloy layers And preparation method thereof, to greatly improve the wear-resisting property of powder metallurgy toothed wheel surface.
To achieve the above object, the technical solution adopted by the present invention are as follows:
A kind of preparation method of Ti (C, N)/Cr (C, N) complex gradient wear-resistant alloy layer comprising the steps of:
(1) C, N strengthening layer are injected in powder metallurgical gear surface ion;
(2) strengthen the double brightness plasma alloying methods of layer surface in C, N and prepare Ti-Cr alloy-layer.
The step (1) comprises the steps of:
(1.1) powder metallurgical gear is ultrasonically treated, gear is immersed in alcohol or acetone, carry out 1~2 ultrasound Then cleaning, 20~30min per treatment are dried;
(1.2) powder metallurgical gear is put into ion implantation device chamber, is passed through argon gas, to through alcohol or acetone cleaning Powder metallurgical gear afterwards carries out 20~30min of pre-sputter cleaning;
(1.3) in vacuum degree less than 2 × 10-3The processing of C, N ion implanting is carried out under the conditions of Pa, injection length is 0.5~2 small When;
(1.4) gear is taken out after furnace is cold, and is saved at room temperature.
In the step (1.2), pre-sputtering parameter is as follows: voltage is 500~700V, beam current density is 0.2~0.4 μ A/ cm2, argon plasma volume density be 1 × 109~3 × 109cm-3
In the step (1.3), the technological parameter of C, N ion implanting processing is as follows: nitrogen gas purity 99.99%, N injection Dosage is 1 × 1017~2 × 1017ions/cm2, C implantation dosage is 4 × 1017~6 × 1017ions/cm2
The step (2) comprises the steps of:
(2.1) after the Ti-Cr target sand paper prepared by powder metallurgic method being polished step by step, immerse in alcohol or acetone into Row 20~30min of ultrasonic cleaning, air-dries and is placed in double brightness device furnaces;
(2.2) interpolar is adjusted away from that is, furnace is closed to 15~18mm at a distance from gear upper surface in Ti-Cr target lower surface Cover, vent valve, breather valve;
(2.3) mechanical pump is opened, evacuating valve is then opened, is evacuated to 10-3Pa is hereinafter, close extraction valve;
(2.4) argon bottle is opened, argon gas valve is opened, flowmeter is then opened and is passed through argon gas, carry out gas washing processing, work as dress When setting air pressure and reaching 145~160Pa, opens vacuum valve and close argon flow valve, air pressure is made to be down to 35~40Pa, repeat The above scrubbing procedure 3~5 times;
(2.5) air pressure is adjusted to 30~40Pa of operating air pressure;
(2.6) 40~50 DEG C of recirculated waters are opened;
(2.7) workpiece pole power supply is opened, using hollow cathode effect build-up of luminance, after aura is stablized, gradually by source voltage tune For 500~600V, workpiece pole tension is adjusted to 300~400V, carries out 0.5h or more to gear and bombards;
(2.8) workpiece pole tension and source voltage are gradually adjusted, until source voltage is 900~1000V, workpiece pole tension For 500~600V.
(2.9) 2.5~3.5 hours are kept the temperature;
(2.10) it gradually slowly reduces source electrode and workpiece pole tension is 0, to avoid stress from concentrating, the time is in 0.5h or more;
(2.11) argon gas valve, vacuum valve, mechanical pump, power switch, circulation taps are closed;
(2.12) 2 hours cooling or more rear taking-up gear.
The mass fraction of Ti is 50~60wt% in the Ti-Cr target, and the mass fraction of Cr is 40~50wt%.
A kind of Ti (C, N)/Cr (C, N) complex gradient wear-resistant alloy layer prepared using the above method, from top to bottom successively Including Ti-Cr sedimentary, Ti (C, N)/Cr (C, N) graded ceramics layer and C, N strengthening layer.
The Ti-Cr sedimentary with a thickness of 15~20 μm, Ti (C, N)/Cr (C, N) graded ceramics layer, C, N strengthening layer Overall thickness is 3~6 μm.
From outward appearance to inner essence gradient declines the Ti (C, N)/Cr (C, N) gradient layer Ti, Cr content, and N content is from outward appearance to inner essence terraced Degree rises.
The utility model has the advantages that the present invention injects ions into conjunction with double brightness plasma alloying technologies, have for preparing one kind The ceramic wear-resisting alloy-layer of composite construction.Since C, N easily interact with alloying element, TiC, CrC of generation, TiN, CrN is metallic bond combination, and bond strength is high, and coefficient of friction is low, and wear-resisting property is good.Therefore first in gear surface ion implanting C, secondly N prepares graded ceramics wear-resistant alloy layer using double brightness plasma alloying technologies, the method can greatly improve powder smelting The wear-resisting property of golden gear surface, prolongs the service life.It has the advantage that
1. after implanting C, N, forming implanted layer in gear surface, surface microstructure is refined, and gear is ground when being on active service Damage amount reduces, and improves the state of abrasive wear.
2. the wear-resistant alloy layer using double brightness plasma alloying technology preparations includes Ti-Cr sedimentary, Ti (C, N)/Cr (C, N) ceramic layer and implanting C, N layer.Ti-Cr layers be ion bombardment sputtering depositing layer, dense structure, no hole and crackle, Greatly improve the wearability of gear.It reacts after C, N of ion implanting and Ti, Cr diffusion of sputtering, formation Ti (C, N)/ Cr (C, N) ceramic layer, ingredient distribution gradient, and be metallurgical bonding with gear, bond strength is high, not easily to fall off.
3. the characteristics of each layer of the Ti (C, N)/Cr (C, N) composite construction graded ceramics wear-resistant alloy layer, is as follows: (1) .Ti- Cr sedimentary is thicker, and the lubricating action of flexible film has been played in friction;(2) Ti (C, N)/Cr (C, N) ceramic layer hardness compared with Height further improves the wear-resisting property of composite construction alloy-layer;(3) implanting C, N strengthening layer make ceramic layer and matrix Between realize without interfaces transition connect, meanwhile, hardness be higher than matrix, be also conducive to promoted matrix wear-resisting property.To sum up, have The wear-resistant alloy layer significant increase of this composite construction wear-resisting property and service life of powder metallurgical gear.
4. due to improve wear-resisting property monotechnics there are respective problems, such as: single ion implantation, implanted layer Thin, wearability promotion is limited, thus causes service life of the implanted layer under operating condition shorter;Simple double brightness plasma alloying technologies Temperature is higher, is likely to result in gear shifting quadrant texturing, influences on its institutional framework, declines the overall performance of gear.Therefore originally Invention injects ions into conjunction with double brightness plasma alloying technologies, is used to prepare a kind of compound with Ti (C, N)/Cr (C, N) The graded ceramics wear-resistant alloy layer of structure.The invention overcomes problem above existing for monotechnics, and it is excellent to realize two kinds of technologies Gesture maximizes, and the wear-resisting property of powder metallurgical gear is greatly improved, substantially extends the service life of gear
Detailed description of the invention
Fig. 1 is Ti (C, N)/Cr (C, N) gradient wear-resistant alloy layer schematic diagram.
Fig. 2 is the SEM figure for the composite construction gradient wear-resistant alloy layer that embodiment 1 obtains.
Specific embodiment
Below with reference to embodiment, invention is further described in detail.But to those skilled in the art, completely Reasonable generalization and derivation can be carried out on the basis of numerical value listed by specific embodiment.
The purity of argon gas used below is that the purity of 99.99%, C is that the purity of 99.99%, Ti is The purity of 99.99%, Cr are 99.99%.Ion implantation device used in following embodiment is the limited public affairs of Beijing Tai Kenuo The LZX-700 high-energy metals ion implantation device (MEVVA ion source) of production is taken charge of, double brightness plasma alloying experiments are using voluntarily It develops, double brightness plasma surface metallurgic equipment of commission Chinese Academy of Sciences Shenyang scientific instrument development center Co., Ltd manufacture.
Embodiment 1
(1) implanting C, N:
(1.1) powder metallurgical gear is ultrasonically treated, gear is immersed in alcohol, carry out 1 ultrasonic cleaning, every time 30min is handled, the impurity on surface is removed, is then dried;
(1.2) gear is put into ion implantation device chamber, is passed through argon gas, to powder metallurgy toothed after alcohol washes Wheel carries out pre-sputter cleaning 30min, and setting parameter is as follows: voltage 500V, beam current density are 0.2 μ A/cm2, argon plasma Density is 1 × 109cm-3
(1.3) start the processing of C, N ion implanting, setting technological parameter is as follows: vacuum degree is lower than 2 × 10-3Pa, nitrogen gas purity It is 1 × 10 for 99.99%, N implantation dosage17ions/cm2, C implantation dosage is 4 × 1017ions/cm2, injection length is 0.5 small When;
(1.4) gear is taken out after furnace is cold, and is saved at room temperature.
(2) Ti-Cr alloy-layer is prepared using double brightness plasma alloying technologies:
(2.1) it after the Ti-Cr target sand paper prepared by powder metallurgy being polished step by step, immerses in alcohol and carries out ultrasonic wave 20min is cleaned, guarantees that surface is pure, air-dries and is placed in double brightness device furnaces;
(2.2) interpolar is adjusted away from that is, Ti-Cr target lower surface is 15mm at a distance from gear upper surface, closes bonnet, puts Air valve, breather valve;
(2.3) mechanical pump is opened, evacuating valve is then opened, is evacuated to 10-3Pa hereinafter, guarantee furnace in vacuum degree, close Close extraction valve;
(2.4) argon bottle is opened, argon gas valve is opened, flowmeter is then opened and is passed through argon gas, carry out gas washing processing;Work as dress When setting air pressure and reaching 150Pa, opens vacuum valve and close argon flow valve, air pressure is made to be down to 40Pa;Repeat the above gas washing Step is three times;
(2.5) air pressure is adjusted to operating air pressure 40Pa;
(2.6) 45 DEG C of recirculated waters are opened;
(2.7) workpiece pole power supply is opened, using hollow cathode effect build-up of luminance, after aura is stablized, gradually by source voltage tune For 500V, workpiece pole tension is adjusted to 300V, and the bombardment of 0.5h is carried out to gear, ion implanting backgear is prevented to be contaminated or send out Raw oxidation;
(2.8) workpiece pole tension and source voltage are gradually adjusted, until source voltage is 920V, workpiece pole tension is 500V;
(2.9) 2.5 hours are kept the temperature;
(2.10) it after terminating heat preservation, gradually slowly reduces source electrode and workpiece pole tension is 0, to avoid stress from concentrating, time In 0.5h or more;
(2.11) argon gas valve, vacuum valve, mechanical pump, power switch, circulation taps are closed;
(2.12) cooling took out gear after 2 hours.
The mass fraction of Ti is 50wt% in Ti-Cr target, and the mass fraction of Cr is 50wt%.Obtained powder metallurgy Gear surface composite construction wear-resistant alloy layer is respectively Ti-Cr sedimentary, Ti (C, N)/Cr (C, N) graded ceramics layer from top to bottom With C, N strengthening layer.Wherein from outward appearance to inner essence gradient declines Ti, Cr content in Ti (C, N)/Cr (C, N) graded ceramics layer, C, N content From outward appearance to inner essence gradient rises.It can be obtained by line scanning, the thickness of Ti-Cr sedimentary is about 15 μm, Ti (C, N)/Cr (C, N) gradient pottery The overall thickness of enamel coating and C, N strengthening layer is 4 μm.
It can be obtained by friction-wear test, the treated more untreated gear of powder metallurgical gear specific wear rate reduces 68.4%.Fig. 2 is the SEM figure of composite construction gradient wear-resistant alloy layer obtained by embodiment 1, wherein I region is Ti-Cr deposition Layer, Ti-Cr layers are ion bombardment sputtering depositing layer, dense structure, no hole and crackle;IIth area is that graded ceramics floor and C, N are strong Change layer, ingredient distribution gradient, and pass through the combination of metallurgical bonding realization and gear, bond strength is high, not easily to fall off.
Embodiment 2
(1) implanting C, N:
(1.1) powder metallurgical gear is ultrasonically treated, in acetone by gear leaching, is cleaned by ultrasonic twice, often Secondary processing 20min, removes the impurity on surface, is then dried;
(1.2) gear is put into ion implantation device chamber, is passed through argon gas, to powder metallurgy toothed after alcohol washes Wheel carries out pre-sputter cleaning 20min, and setting parameter is as follows: voltage 600V, beam current density are 0.3 μ A/cm2, argon plasma Density is 2 × 109cm-3
(1.3) start the processing of C, N ion implanting, setting technological parameter is as follows: vacuum degree is lower than 2 × 10-3Pa, nitrogen gas purity It is 1.5 × 10 for 99.99%, N implantation dosage17ions/cm2, C implantation dosage is 5 × 1017ions/cm2, injection length is 1 small When;
(1.4) gear is taken out after furnace is cold, and is saved at room temperature.
(2) Ti-Cr alloy-layer is prepared using double brightness plasma alloying technologies:
(2.1) it after the Ti-Cr target sand paper prepared by powder metallurgy being polished step by step, immerses in alcohol and carries out ultrasonic wave 30min is cleaned, guarantees that surface is pure, air-dries and is placed in double brightness device furnaces;
(2.2) interpolar is adjusted away from that is, Ti-Cr target lower surface is to 16mm at a distance from gear upper surface, and interpolar is away from meeting shadow Hollow cathode build-up of luminance effect is rung, too small to will lead to aura extinguishing, the excessive alloying element utilization rate that will cause is low, closes bonnet, puts Air valve, breather valve;
(2.3) mechanical pump is opened, evacuating valve is then opened, is evacuated to 10-3Pa hereinafter, guarantee furnace in vacuum degree, close Close extraction valve;
(2.4) argon bottle is opened, argon gas valve is opened, flowmeter is then opened and is passed through argon gas, carry out gas washing processing, argon gas It does not react with the metallic element in target and to sputter ability higher, when device air pressure reaches 145Pa, open vacuum valve simultaneously And argon flow valve is closed, so that air pressure is down to 35Pa, repeats the above scrubbing procedure three times;
(2.5) air pressure is adjusted to operating air pressure 35Pa;
(2.6) 40 DEG C of recirculated waters are opened;
(2.7) workpiece pole power supply is opened, using hollow cathode effect build-up of luminance, after aura is stablized, gradually by source voltage tune For 550V, workpiece pole tension is adjusted to 350V, and the bombardment of 0.5h is carried out to gear, ion implanting backgear is prevented to be contaminated or send out Raw oxidation;
(2.8) workpiece pole tension and source voltage are gradually adjusted, until source voltage is 950V, workpiece pole tension is 550V, in-furnace temperature rise naturally;
(2.9) 3 hours are kept the temperature;
(2.10) it after terminating heat preservation, gradually slowly reduces source electrode and workpiece pole tension is 0, to avoid stress from concentrating, time In 0.5h or more;
(2.11) argon gas valve, vacuum valve, mechanical pump, power switch, circulation taps are closed;
(2.12) cooling took out gear after 4 hours.
The mass fraction of Ti is 60wt% in Ti-Cr target, and the mass fraction of Cr is 40wt%.Obtained powder metallurgy Gear surface composite construction wear-resistant alloy layer is respectively Ti-Cr sedimentary, Ti (C, N)/Cr (C, N) graded ceramics layer from top to bottom With C, N strengthening layer.Wherein from outward appearance to inner essence gradient declines Ti, Cr content in Ti (C, N)/Cr (C, N) graded ceramics layer, C, N content From outward appearance to inner essence gradient rises.It can be obtained by line scanning, the thickness of Ti-Cr sedimentary is about 17 μm, Ti (C, N)/Cr (C, N) gradient pottery The overall thickness of enamel coating and C, N strengthening layer is 5 μm.
It can be obtained by friction-wear test, the treated more untreated gear of powder metallurgical gear specific wear rate reduces 67.25%.
Embodiment 3
(1) implanting C, N:
(1.1) powder metallurgical gear is ultrasonically treated, in acetone by gear leaching, is cleaned by ultrasonic twice, often Secondary processing 25min, removes the impurity on surface, is then dried;
(1.2) gear is put into ion implantation device chamber, is passed through argon gas, to powder metallurgy toothed after alcohol washes Wheel carries out pre-sputter cleaning 25min, and setting parameter is as follows: voltage 700V, beam current density are 0.4 μ A/cm2, argon plasma Density is 3 × 109cm-3
(1.3) start the processing of C, N ion implanting, setting technological parameter is as follows: vacuum degree is lower than 2 × 10-3Pa, nitrogen gas purity It is 2 × 10 for 99.99%, N implantation dosage17ions/cm2, C implantation dosage is 6 × 1017ions/cm2, injection length is 2 small When;
(1.4) gear is taken out after furnace is cold, and is saved at room temperature.
(2) Ti-Cr alloy-layer is prepared using double brightness plasma alloying technologies:
(2.1) it after the Ti-Cr target sand paper prepared by powder metallurgy being polished step by step, immerses in alcohol and carries out ultrasonic wave 25min is cleaned, guarantees that surface is pure, air-dries and is placed in double brightness device furnaces;
(2.2) interpolar is adjusted away from that is, Ti-Cr target lower surface is to 18mm at a distance from gear upper surface, and interpolar is away from meeting shadow Hollow cathode build-up of luminance effect is rung, too small to will lead to aura extinguishing, the excessive alloying element utilization rate that will cause is low, closes bonnet, puts Air valve, breather valve;
(2.3) mechanical pump is opened, evacuating valve is then opened, is evacuated to 10-3Pa hereinafter, guarantee furnace in vacuum degree, close Close extraction valve;
(2.4) argon bottle is opened, argon gas valve is opened, flowmeter is then opened and is passed through argon gas, carry out gas washing processing, argon gas It does not react with the metallic element in target and to sputter ability higher, when device air pressure reaches 160Pa, open vacuum valve simultaneously And argon flow valve is closed, so that air pressure is down to 40Pa, repeats the above scrubbing procedure three times;
(2.5) air pressure is adjusted to operating air pressure 40Pa;
(2.6) 50 DEG C of recirculated waters are opened;
(2.7) workpiece pole power supply is opened, using hollow cathode effect build-up of luminance, after aura is stablized, gradually by source voltage tune For 600V, workpiece pole tension is adjusted to 400V, and the bombardment of 1h is carried out to gear, ion implanting backgear is prevented to be contaminated or occur Oxidation;
(2.8) workpiece pole tension and source voltage are gradually adjusted, until source voltage is 1000V, workpiece pole tension is 600V;
(2.9) 3.5 hours are kept the temperature;
(2.10) it after terminating heat preservation, gradually slowly reduces source electrode and workpiece pole tension is 0, to avoid stress from concentrating, time In 0.5h or more;
(2.11) argon gas valve, vacuum valve, mechanical pump, power switch, circulation taps are closed;
(2.12) cooling took out gear after 5 hours.
The mass fraction of Ti is 60wt% in Ti-Cr target, and the mass fraction of Cr is 40wt%.Obtained powder metallurgy Gear surface composite construction wear-resistant alloy layer is respectively Ti-Cr sedimentary, Ti (C, N)/Cr (C, N) graded ceramics layer from top to bottom With C, N strengthening layer.Wherein from outward appearance to inner essence gradient declines Ti, Cr content in Ti (C, N)/Cr (C, N) graded ceramics layer, C, N content From outward appearance to inner essence gradient rises.It can be obtained by line scanning, the thickness of Ti-Cr sedimentary is about 19 μm, Ti (C, N)/Cr (C, N) gradient pottery The overall thickness of enamel coating and C, N strengthening layer is 6 μm.
It can be obtained by friction-wear test, the treated more untreated gear of powder metallurgical gear specific wear rate reduces 70.34%.
The above is only a preferred embodiment of the present invention, it is noted that for the ordinary skill people of the art For member, various improvements and modifications may be made without departing from the principle of the present invention, these improvements and modifications are also answered It is considered as protection scope of the present invention.

Claims (7)

1. a kind of Ti (C, N)/Cr (C, N) complex gradient wear-resistant alloy layer preparation method, it is characterised in that: include following step It is rapid:
(1) C, N strengthening layer are injected in powder metallurgical gear surface ion;It comprises the steps of:
(1.1) powder metallurgical gear is ultrasonically treated, gear is immersed in alcohol or acetone, carry out 1 ~ 2 ultrasonic cleaning, 20 ~ 30min per treatment, is then dried;
(1.2) powder metallurgical gear is put into ion implantation device chamber, is passed through argon gas, to after alcohol or acetone cleaning Powder metallurgical gear carries out 20 ~ 30min of pre-sputter cleaning;
(1.3) in vacuum degree less than 2 × 10-3The processing of C, N ion implanting is carried out under the conditions of Pa, injection length is 0.5 ~ 2 hour;
(1.4) gear is taken out after furnace is cold, and is saved at room temperature;
(2) strengthen the double brightness plasma alloying methods of layer surface in C, N and prepare Ti-Cr alloy-layer;It comprises the steps of:
(2.1) it after the Ti-Cr target sand paper prepared by powder metallurgic method being polished step by step, immerses in alcohol or acetone and is surpassed Sound cleans 20 ~ 30min, air-dries and is placed in double brightness device furnaces;
(2.2) interpolar is adjusted away from that is, Ti-Cr target lower surface is closed bonnet, put to 15 ~ 18mm at a distance from gear upper surface Air valve, breather valve;
(2.3) mechanical pump is opened, evacuating valve is then opened, is evacuated to 10-3Pa is hereinafter, close extraction valve;
(2.4) argon bottle is opened, argon gas valve is opened, flowmeter is then opened and is passed through argon gas, gas washing processing is carried out, when device gas It when pressure reaches 145 ~ 160Pa, opens vacuum valve and closes argon flow valve, air pressure is made to be down to 35 ~ 40Pa, repeat above wash Jia bombardier rapid 3 ~ 5 times;
(2.5) air pressure is adjusted to 30 ~ 40Pa of operating air pressure;
(2.6) 40 ~ 50 DEG C of recirculated waters are opened;
(2.7) workpiece pole power supply is opened, source voltage is gradually adjusted to 500 after aura is stablized using hollow cathode effect build-up of luminance ~ 600V, workpiece pole tension are adjusted to 300 ~ 400V, carry out 0.5h or more to gear and bombard;
(2.8) workpiece pole tension and source voltage are gradually adjusted, until source voltage is 900 ~ 1000V, workpiece pole tension is 500 ~600V;
(2.9) 2.5 ~ 3.5 hours are kept the temperature;
(2.10) it gradually slowly reduces source electrode and workpiece pole tension is 0, to avoid stress from concentrating, the time is in 0.5h or more;
(2.11) argon gas valve, vacuum valve, mechanical pump, power switch, circulation taps are closed;
(2.12) 2 hours cooling or more rear taking-up gear.
2. Ti (C, N) according to claim 1/Cr (C, N) complex gradient wear-resistant alloy layer preparation method, feature exist In: in the step (1.2), pre-sputtering parameter is as follows: voltage is 500~700V, beam current density is 0.2 ~ 0.4 μ A/cm2, argon Plasma density is 1 × 109~3 × 109cm-3
3. Ti (C, N) according to claim 1/Cr (C, N) complex gradient wear-resistant alloy layer preparation method, feature exist In: in the step (1.3), the technological parameter of C, N ion implanting processing is as follows: nitrogen gas purity 99.99%, N implantation dosage It is 1 × 1017~2×1017ions/cm2, C implantation dosage is 4 × 1017~6×1017ions/cm2
4. Ti (C, N) according to claim 1/Cr (C, N) complex gradient wear-resistant alloy layer preparation method, feature exist In: the mass fraction of Ti is 50 ~ 60wt% in the Ti-Cr target, and the mass fraction of Cr is 40 ~ 50wt%.
5. a kind of Ti (C, N)/Cr (C, N) complex gradient antifriction alloy using any method preparation of claim 1 ~ 4 Layer, it is characterised in that: from top to bottom successively include that Ti-Cr sedimentary, Ti (C, N)/Cr (C, N) graded ceramics layer and C, N strengthen Layer.
6. Ti (C, N) according to claim 5/Cr (C, N) complex gradient wear-resistant alloy layer, it is characterised in that: the Ti- Cr sedimentary with a thickness of 15 ~ 20 μm, Ti (C, N)/Cr (C, N) graded ceramics layer, C, N strengthening layer overall thickness be 3 ~ 6 μm.
7. Ti (C, N) according to claim 5/Cr (C, N) complex gradient wear-resistant alloy layer, it is characterised in that: the Ti From outward appearance to inner essence gradient declines Ti, Cr content of (C, N)/Cr (C, N) gradient layer, and from outward appearance to inner essence gradient rises for C, N content.
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