CN109306464A - A kind of graded ceramics wear-resistant alloy layer of Ti/CrN composite construction and preparation method thereof - Google Patents

A kind of graded ceramics wear-resistant alloy layer of Ti/CrN composite construction and preparation method thereof Download PDF

Info

Publication number
CN109306464A
CN109306464A CN201811055964.0A CN201811055964A CN109306464A CN 109306464 A CN109306464 A CN 109306464A CN 201811055964 A CN201811055964 A CN 201811055964A CN 109306464 A CN109306464 A CN 109306464A
Authority
CN
China
Prior art keywords
layer
gear
wear
crn
composite construction
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Granted
Application number
CN201811055964.0A
Other languages
Chinese (zh)
Other versions
CN109306464B (en
Inventor
魏东博
张平则
梁宏璇
刘子利
李淑琴
姚正军
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Nanjing University of Aeronautics and Astronautics
Original Assignee
Nanjing University of Aeronautics and Astronautics
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Nanjing University of Aeronautics and Astronautics filed Critical Nanjing University of Aeronautics and Astronautics
Priority to CN201811055964.0A priority Critical patent/CN109306464B/en
Publication of CN109306464A publication Critical patent/CN109306464A/en
Application granted granted Critical
Publication of CN109306464B publication Critical patent/CN109306464B/en
Active legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Classifications

    • 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
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F3/00Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
    • B22F3/24After-treatment of workpieces or articles
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F5/00Manufacture of workpieces or articles from metallic powder characterised by the special shape of the product
    • B22F5/08Manufacture of workpieces or articles from metallic powder characterised by the special shape of the product of toothed articles, e.g. gear wheels; of cam discs
    • 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
    • CCHEMISTRY; METALLURGY
    • C23COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23CCOATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/22Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
    • C23C14/24Vacuum evaporation
    • C23C14/32Vacuum evaporation by explosion; by evaporation and subsequent ionisation of the vapours, e.g. ion-plating
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F3/00Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
    • B22F3/24After-treatment of workpieces or articles
    • B22F2003/241Chemical after-treatment on the surface
    • B22F2003/242Coating

Abstract

The invention discloses graded ceramics wear-resistant alloy layer of a kind of Ti/CrN composite construction and preparation method thereof, which successively includes Ti-Cr sedimentary, Ti/CrN graded ceramics layer and N strengthening layer from top to bottom.Preparation method are as follows: (1) inject N strengthening layer in powder metallurgical gear surface ion;(2) strengthen the double brightness plasma alloying methods of layer surface in N and prepare Ti-Cr alloy-layer.Nitrogen-atoms easily interacts with alloying element, and wear-resisting property can be improved in the nitride of formation.During plasma alloying, the N of Ti, Cr ion sputtered and ion implanting reacts, and forms the graded ceramics wear-resistant alloy layer of Ti/CrN composite construction.Compared to the method that other improve powder metallurgical gear wear-resisting property, the present invention realizes two kinds of technical advantages and maximizes, greatly improves the wear-resisting property of powder metallurgical gear, extend the service life of gear.

Description

A kind of graded ceramics wear-resistant alloy layer of Ti/CrN composite construction 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/CrN composite construction Graded ceramics wear-resistant alloy layer and its preparation process.
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. Conventional machining process generallys use this mode, but Integral alloy chemical industry skill is at high cost, pollutes larger;Second is that passing through advanced table Face modification technology forms modified layer on driven gears surface, improves the wear-resisting property of gear.Abrasion is usually to open from material surface Begin, therefore is a kind of more common method by the modified wear-resisting property to improve gear in surface.These process for modifying surface It mainly include carburizing, nitriding, carbo-nitriding, thermal spraying, ion implanting, vacuum ion plating etc..It is prepared using hot-spraying technique Coating and gear are in mechanical bond, and bond strength is low, is easy to appear hole, micro-crack, disbonding etc. in use and asks Topic, reduces the bond strength of coating and gear;Ion implantation technology can will improve the ion of the element of wear-resisting property in vacuum It is injected in gear in system, to form the implanted layer that wear-resisting property is improved.But ion implanted layer thickness is not high, and can only Straight line injection is carried out, the wear-resisting property of gear cannot be improved comprehensively;The surface alloying layer of double brightness plasma alloying technology preparations Including alloy-layer and diffusion layer, ingredient, performance are distributed with concentration gradient, are firmly combined with matrix, and alloy-layer dense structure, nothing The defects of gap, crackle, work efficiency 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.
" the heat processing technique " " shadow of density to Multlelement Co-Penetrated Layer of Iron Base P/M published in 1997 Sound " one is disclosed herein a kind of wear-resisting to improve powdered metallurgical material for the multi element copermeation technology of main penetration enhancer with methanol and urea The method of performance;" optical-mechanical " the 3rd published for 1988 is interim, and " laser treatment improves grinding for powdered metallurgical material wear-resisting property Study carefully " one be disclosed herein using laser treatment improve powdered metallurgical material wearability method;" the Jiangsu science and technology published for 2009 College journal: natural science edition " interim " the gear surface Current Status of Modification " one of volume 23 the 2nd be disclosed herein using true The method of coating Ni-W and Ni-CO alloy coat can compared with non-coating on the HT250 cast iron gear flank of tooth for empty ion plating To improve the abrasion resistance properties of cast iron gear up to 4~6 times." vacuum science and the Technology " published volume 30 the 3rd in 2010 Use is disclosed herein in interim " ion implanting space gear driving pair 30CrMnSi material vacuum tribological Properties " one Ion implanting injects Ti, C, N element on gear, the method for improving gear wear-resisting property.But the shortcomings that ion implantation technique, is It is insufficient to inject layer depth, thickness is small, and which also limits its applications on gear surface reinforcement technique." the Shen published in 2013 Positive engineering college's journal: natural science edition " interim " the power station coal pulverizer gear wear Research on application of protection technique " one of volume 9 the 1st The method for improving gear surface wear-resisting property using plasma spray technology is disclosed herein.But the coating of technique preparation is in gear The problems such as mechanical bond, bond strength is low, is easy to appear hole, micro-crack, disbonding in use, reduces coating With the bond strength of gear." rare metal and hard alloy " interim " double brightness plasma Cr- of volume 39 the 3rd published in 2011 Si permeation improvement γ-TiAl-base alloy wear-resisting property research " one is disclosed herein using double brightness plasma alloying technology systems The method that standby Cr-Si infiltration layer improves matrix wear-resisting property.
Since powder metallurgical gear wear-resisting property is difficult to meet 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;Simple double brightness plasma alloying technology temperature are higher, gear shifting quadrant texturing are likely to result in, to it Institutional framework has an impact, 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 process temperature is higher, is likely to result in gear shifting quadrant texturing, has an impact, makes under the overall performance of gear to its institutional framework Drop.
Summary of the invention
In view of the above problems, the object of the present invention is to provide a kind of graded ceramics wear-resistant alloy layers of Ti/CrN composite construction And preparation method thereof, which can greatly improve the wear-resisting property of powder metallurgy toothed wheel surface, prolong its service life.
To achieve the above object, the technical solution adopted by the present invention are as follows:
A kind of preparation method of the graded ceramics wear-resistant alloy layer of Ti/CrN composite construction comprising the steps of:
(1) N strengthening layer is injected in powder metallurgical gear surface ion;
(2) strengthen the double brightness plasma alloying methods of layer surface in 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 10-3The processing of N ion implanting is carried out under the conditions of Pa, injection length is 0.5~1.5 hour;
(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 N ion implanting processing is as follows: nitrogen gas purity 99.99%, Nitrogen ion Injecting voltage is 30~50kV, and beam current density is 2~2.5 μ A/cm2, nitrogen plasma density is 1 × 109~3 × 109cm-3, note Entering dosage is 3 × 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 18~20mm 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 300~450V, 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 900~940V, workpiece pole tension For 520~550V.
(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 60~70wt% in the Ti-Cr target, and the mass fraction of Cr is 30~40wt%.
A kind of graded ceramics wear-resistant alloy layer of the Ti/CrN composite construction using above method preparation, from top to bottom successively Including Ti-Cr sedimentary, Ti/CrN graded ceramics layer and N strengthening layer.
The Ti-Cr sedimentary with a thickness of 15~20 μm, Ti/CrN graded ceramics layer, N strengthening layer overall thickness be 3~ 6μm。
From outward appearance to inner essence gradient declines Ti, Cr content of the Ti/CrN gradient layer, and from outward appearance to inner essence gradient rises N content.
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 Ti/CrN composite construction.First in gear surface ion implanting N, double brightness plasma alloys are secondly utilized Change technology prepares graded ceramics wear-resistant alloy layer.The method can greatly improve the wear-resisting property of powder metallurgy toothed wheel surface, extend Its service life.It has the advantage that
1. after ion implanting N, forming implanted layer in gear surface, having refined surface microstructure, wear-resisting property is centainly mentioned It rises.
2.Ti-Cr layers are ion bombardment sputtering depositing layer, and the layer tissue is fine and close, no hole and crackle.The N of ion implanting with It reacts after Ti, Cr diffusion of sputtering, forms Ti/CrN ceramic layer, ingredient, performance are distributed with concentration gradient, are with gear Metallurgical bonding, bond strength is high, not easily to fall off.
3. the effect in each region of graded ceramics wear-resistant alloy layer of the Ti/CrN composite construction is respectively as follows: (1) Ti-Cr deposition Layer has played the lubricating action of flexible film in friction, reduces coefficient of friction, improves wear-resisting property;(2) Ti/CrN makes pottery Enamel coating hardness is higher, further improves the wear-resisting property of composite construction alloy-layer;(3) ion implanting N strengthening layer makes ceramics It realizes between layer and matrix and is connected without interfaces transition, meanwhile, hardness is higher than matrix, is also conducive to the wear-resisting property for promoting matrix. To sum up, it the wear-resisting property of the gradient wear-resistant alloy layer significant increase of Ti/CrN composite construction powder metallurgical gear and is on active service the longevity Life.
4. due to improve wear-resisting property monotechnics there are respective problems: single ion implantation, implanted layer is thin, Wearability promotion is limited, thus causes service life of the implanted layer under operating condition shorter;Simple double brightness plasma alloying technology temperature Degree is higher, is likely to result in gear shifting quadrant texturing, has an impact to its institutional framework, declines the overall performance of gear.The present invention will It is resistance to be used to prepare a kind of graded ceramics with Ti/CrN composite construction in conjunction with double brightness plasma alloying technologies for ion implanting Merge layer gold.The invention overcomes problem above existing for monotechnics, realizes two kinds of technical advantages and maximizes, is greatly improved The wear-resisting property of powder metallurgical gear substantially extends the service life of gear.
Detailed description of the invention
Fig. 1 is the gradient wear-resistant alloy layer schematic diagram of Ti/CrN composite construction.
Fig. 2 is the SEM figure for the composite construction gradient wear-resistant alloy layer that embodiment 1 is prepared.
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%, Ti is that the purity of 99.99%, Cr is 99.99%.Ion implantation device used in following embodiment is the LZX-700 high energy gold of Beijing Tai Kenuo Co., Ltd production Belong to ion implantation device (MEVVA ion source), double brightness plasma alloying experiments entrust Chinese Academy of Sciences Shenyang section using voluntarily developing Learn double brightness plasma surface metallurgic equipment of instrument development centered finite company manufacture.
Embodiment 1
(1) ion implanting N:
(1.1) powder metallurgical gear is ultrasonically treated, gear is immersed in alcohol, be cleaned by ultrasonic twice, often Secondary processing 30min, 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 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 N ion implanting, setting technological parameter is as follows: vacuum degree is lower than 10-3Pa, nitrogen gas purity are 99.99%, N~+ implantation voltage is 35kV, and beam current density is 2 μ A/cm2, nitrogen plasma density is 1 × 109cm-3, injection Dosage is 3 × 1017ions/cm2, injection length is 1 hour;
(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 closed bonnet, put to 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 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 900V, workpiece pole tension is 520V;(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 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 from top to bottom, and Ti/CrN graded ceramics layer and N strengthen Layer.Wherein from outward appearance to inner essence gradient declines Ti, Cr content in Ti/CrN graded ceramics layer, and from outward appearance to inner essence gradient rises N content.By line Scanning can obtain, and the thickness of Ti-Cr sedimentary is about 15 μm, and the overall thickness of Ti/CrN graded ceramics layer and 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 N strengthen 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) ion implanting N:
(1.1) powder metallurgical gear is ultrasonically treated, gear is immersed in alcohol, be 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 N ion implanting, setting technological parameter is as follows: vacuum degree is lower than 10-3Pa, nitrogen gas purity are 99.99%, N~+ implantation voltage is 45kV, and beam current density is 2.2 μ A/cm2, nitrogen plasma density is 2 × 109cm-3, note Entering dosage is 5 × 1017ions/cm2, injection length is 1.5 hours.
(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 closed bonnet, put to 19mm 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 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 550V, workpiece pole tension is adjusted to 400V, and the low temperature for carrying out 0.5h to gear bombards, and ion implanting backgear is prevented to be contaminated Or it aoxidizes;
(2.8) workpiece pole tension and source voltage are gradually adjusted, until source voltage is 920V, workpiece pole tension is 540V;
(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 from top to bottom, and Ti/CrN graded ceramics layer and N strengthen Layer.Wherein from outward appearance to inner essence gradient declines Ti, Cr content in Ti/CrN graded ceramics layer, and from outward appearance to inner essence gradient rises N content.By line Scanning can obtain, and the thickness of Ti-Cr sedimentary is about 17 μm, and the overall thickness of Ti/CrN graded ceramics layer and 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 72.4%.
Embodiment 3
(1) ion implanting N:
(1.1) powder metallurgical gear is ultrasonically treated, in acetone by gear leaching, carries out 1 ultrasonic cleaning, 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 acetone cleans 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 N ion implanting, setting technological parameter is as follows: vacuum degree is lower than 10-3Pa, nitrogen gas purity are 99.99%, N~+ implantation voltage is 50kV, and beam current density is 2.5 μ A/cm2, nitrogen plasma density is 3 × 109cm-3, note Entering dosage is 6 × 1017ions/cm2, injection length is 1.5 hours;
(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 closed bonnet, put to 20mm 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 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 35Pa, repeat the above gas washing Step 5 time;
(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 600V, workpiece pole tension is adjusted to 450V, to gear carry out 1h low temperature bombard, prevent ion implanting backgear be contaminated or It aoxidizes;
(2.8) workpiece pole tension and source voltage are gradually adjusted, until source voltage is 940V, workpiece pole tension is 550V;
(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 70wt% in Ti-Cr target, and the mass fraction of Cr is 30wt%.Obtained powder metallurgy Gear surface composite construction wear-resistant alloy layer is respectively Ti-Cr sedimentary from top to bottom, and Ti/CrN graded ceramics layer and N strengthen Layer.Wherein from outward appearance to inner essence gradient declines Ti, Cr content in Ti/CrN graded ceramics layer, and from outward appearance to inner essence gradient rises N content.By line Scanning can obtain, and the thickness of Ti-Cr sedimentary is about 19 μm, and the overall thickness of Ti/CrN graded ceramics layer and 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 73.2%.
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 (9)

1. a kind of preparation method of the graded ceramics wear-resistant alloy layer of Ti/CrN composite construction, it is characterised in that: include following step It is rapid:
(1) N strengthening layer is injected in powder metallurgical gear surface ion;
(2) strengthen the double brightness plasma alloying methods of layer surface in N and prepare Ti-Cr alloy-layer.
2. the preparation method of the graded ceramics wear-resistant alloy layer of Ti/CrN composite construction according to claim 1, feature Be: the step (1) comprises the steps of:
(1.1) powder metallurgical gear is ultrasonically treated, gear is immersed in alcohol or acetone, it is clear to carry out 1~2 ultrasound It washes, then 20~30min per treatment is 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 10-3The processing of N ion implanting is carried out under the conditions of Pa, injection length is 0.5~1.5 hour;
(1.4) gear is taken out after furnace is cold, and is saved at room temperature.
3. the preparation method of the graded ceramics wear-resistant alloy layer of Ti/CrN composite construction according to claim 2, feature Be: 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 is 1 × 109~3 × 109cm-3
4. the preparation method of the graded ceramics wear-resistant alloy layer of Ti/CrN composite construction according to claim 2, feature Be: in the step (1.3), the technological parameter of N ion implanting processing is as follows: nitrogen gas purity 99.99%, N~+ implantation Voltage is 30~50kV, and beam current density is 2~2.5 μ A/cm2, nitrogen plasma density is 1 × 109~3 × 109cm-3, injectant Amount is 3 × 1017~6 × 1017ions/cm2
5. the preparation method of the graded ceramics wear-resistant alloy layer of Ti/CrN composite construction according to claim 1, feature Be: the step (2) 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 18~20mm 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 Pressure opens vacuum valve and closes argon flow valve, air pressure is made to be down to 35~40Pa when reaching 145~160Pa, repeat more than 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, 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 300~450V, 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 900~940V, workpiece pole tension is 520 ~550V.
(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.
6. the preparation method of the graded ceramics wear-resistant alloy layer of Ti/CrN composite construction according to claim 5, feature Be: the mass fraction of Ti is 60~70wt% in the Ti-Cr target, and the mass fraction of Cr is 30~40wt%.
7. a kind of resistance to adjustment of graded ceramics of the Ti/CrN composite construction using any method preparation of claim 1~6 Layer gold, it is characterised in that: from top to bottom successively include Ti-Cr sedimentary, Ti/CrN graded ceramics layer and N strengthening layer.
8. the graded ceramics wear-resistant alloy layer of Ti/CrN composite construction according to claim 7, it is characterised in that: described Ti-Cr sedimentary with a thickness of 15~20 μm, Ti/CrN graded ceramics layer, N strengthening layer overall thickness be 3~6 μm.
9. the graded ceramics wear-resistant alloy layer of Ti/CrN composite construction according to claim 7, it is characterised in that: described From outward appearance to inner essence gradient declines Ti, Cr content of Ti/CrN gradient layer, and from outward appearance to inner essence gradient rises N content.
CN201811055964.0A 2018-09-11 2018-09-11 Gradient ceramic wear-resistant alloy layer with Ti/CrN composite structure and preparation method thereof Active CN109306464B (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201811055964.0A CN109306464B (en) 2018-09-11 2018-09-11 Gradient ceramic wear-resistant alloy layer with Ti/CrN composite structure and preparation method thereof

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201811055964.0A CN109306464B (en) 2018-09-11 2018-09-11 Gradient ceramic wear-resistant alloy layer with Ti/CrN composite structure and preparation method thereof

Publications (2)

Publication Number Publication Date
CN109306464A true CN109306464A (en) 2019-02-05
CN109306464B CN109306464B (en) 2019-12-24

Family

ID=65224712

Family Applications (1)

Application Number Title Priority Date Filing Date
CN201811055964.0A Active CN109306464B (en) 2018-09-11 2018-09-11 Gradient ceramic wear-resistant alloy layer with Ti/CrN composite structure and preparation method thereof

Country Status (1)

Country Link
CN (1) CN109306464B (en)

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111020516A (en) * 2019-11-22 2020-04-17 中国航发西安动力控制科技有限公司 Method for improving self-lubricating property of oil distributing valve
CN114570929A (en) * 2022-03-04 2022-06-03 盐城东葵科技有限公司 Heavy-load anti-fatigue reduction gear and preparation method thereof

Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1122380A (en) * 1995-08-25 1996-05-15 北京有色金属研究总院 Composite surface treatment method for steel die
CN106342102B (en) * 2006-12-27 2010-12-15 上海航天设备制造总厂 The comprehensive ion implantation and deposition complex intensifying processing method in titanium alloy component surface
CN103775634A (en) * 2014-02-21 2014-05-07 四川金星压缩机制造有限公司 Composite coating piston rod and manufacturing method thereof
CN104561909A (en) * 2015-01-27 2015-04-29 大连理工常州研究院有限公司 Ionitriding/arc ion plating surface composite modification apparatus and method
CN107326360A (en) * 2017-07-13 2017-11-07 西安交通大学 A kind of erosion resistant coating structure of nanometer multilayer graded composite and preparation method thereof

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1122380A (en) * 1995-08-25 1996-05-15 北京有色金属研究总院 Composite surface treatment method for steel die
CN106342102B (en) * 2006-12-27 2010-12-15 上海航天设备制造总厂 The comprehensive ion implantation and deposition complex intensifying processing method in titanium alloy component surface
CN103775634A (en) * 2014-02-21 2014-05-07 四川金星压缩机制造有限公司 Composite coating piston rod and manufacturing method thereof
CN104561909A (en) * 2015-01-27 2015-04-29 大连理工常州研究院有限公司 Ionitriding/arc ion plating surface composite modification apparatus and method
CN107326360A (en) * 2017-07-13 2017-11-07 西安交通大学 A kind of erosion resistant coating structure of nanometer multilayer graded composite and preparation method thereof

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111020516A (en) * 2019-11-22 2020-04-17 中国航发西安动力控制科技有限公司 Method for improving self-lubricating property of oil distributing valve
CN114570929A (en) * 2022-03-04 2022-06-03 盐城东葵科技有限公司 Heavy-load anti-fatigue reduction gear and preparation method thereof
CN114570929B (en) * 2022-03-04 2024-04-02 盐城东葵科技有限公司 Heavy-load anti-fatigue type speed reduction gear coating tool

Also Published As

Publication number Publication date
CN109306464B (en) 2019-12-24

Similar Documents

Publication Publication Date Title
CN102732832B (en) Titanium alloy surface high temperature oxidation resistance and wear resistance oxide gradient coat, and preparation method thereof
CN104746030A (en) Method for improving bonding strength of hard alloy and diamond coating
CN101532122B (en) Method for preparing diamond-like coating on surface of biological medical NiTi alloy
CN106702329A (en) Multi-arc ion-plating-aluminum based micro-arc oxidation ceramic coating on titanium alloy surface and preparation method of multi-arc ion-plating-aluminum based micro-arc oxidation ceramic coating
CN102732833B (en) Gamma-TiAl alloy surface high temperature oxidation resistance and wear resistance coat, and preparation method thereof
CN109338323B (en) A kind of raising Al2O3The surface treatment method of ceramics and Nickel-based Alloy Welding performance
CN109898064A (en) A kind of DLC/Me-C laminated film and preparation method thereof
CN107937875A (en) A kind of preparation method of Sintered NdFeB magnet surface protection coating
CN109306464A (en) A kind of graded ceramics wear-resistant alloy layer of Ti/CrN composite construction and preparation method thereof
CN109929986A (en) A kind of composite material and preparation method
CN101709470A (en) Preparation method of composite coating containing diffusion barrier generated in situ
CN109023249B (en) A kind of raising powder metallurgical gear surface abrasion resistance alloy-layer and preparation method thereof
CN109706503A (en) A kind of the antibacterial wear-resistant coating and preparation method on Titanium base surface
CN109023285B (en) A kind of Ti (C, N)/Cr (C, N) complex gradient wear-resistant alloy layer and preparation method thereof
CN105734487A (en) Method for preparing tough molybdenum gradient modified layer on surface of titanium alloy gear
CN104532197A (en) Composite coating prepared through ion implantation of Al on steel surface after double-glow Cr alloying and preparation method of composite coating
CN104087902A (en) Insulating coating on surface of metal material and preparation method of insulating coating
CN109161865B (en) A kind of raising Si3N4The surface treatment method of ceramics and gamma-TiAl alloy welding performance
CN109023286B (en) Composite gradient wear-resistant alloy layer and preparation method thereof
CN104532189A (en) Fine Sn phase AlSn20Cu coating for bearing bush and preparation method thereof
CN105112862B (en) The material and preparation method of gadolinium copper alloy layer are formed on pure gadolinium surface
CN105463372B (en) A kind of preparation method of MULTILAYER COMPOSITE super thick self-lubricating hard coating
CN106756827B (en) A kind of process of surface treatment of jewellery rigid pure gold
CN108070859A (en) Refractory metal surfaces lamellar composite Ir/W high-temperature oxidation resistant coatings and preparation method thereof
CN107267934B (en) A kind of screw in injection molding machine surface reinforcing method

Legal Events

Date Code Title Description
PB01 Publication
PB01 Publication
SE01 Entry into force of request for substantive examination
SE01 Entry into force of request for substantive examination
GR01 Patent grant
GR01 Patent grant