CN109306464B - Gradient ceramic wear-resistant alloy layer with Ti/CrN composite structure and preparation method thereof - Google Patents
Gradient ceramic wear-resistant alloy layer with Ti/CrN composite structure and preparation method thereof Download PDFInfo
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- 229910045601 alloy Inorganic materials 0.000 title claims abstract description 40
- 239000000956 alloy Substances 0.000 title claims abstract description 40
- 239000000919 ceramic Substances 0.000 title claims abstract description 39
- 239000002131 composite material Substances 0.000 title claims abstract description 26
- 238000002360 preparation method Methods 0.000 title claims abstract description 8
- 238000004663 powder metallurgy Methods 0.000 claims abstract description 44
- 238000000034 method Methods 0.000 claims abstract description 38
- 238000005275 alloying Methods 0.000 claims abstract description 21
- 238000005728 strengthening Methods 0.000 claims abstract description 20
- 230000008569 process Effects 0.000 claims abstract description 13
- 229910052804 chromium Inorganic materials 0.000 claims abstract description 8
- 229910000599 Cr alloy Inorganic materials 0.000 claims abstract description 6
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 75
- 229910052786 argon Inorganic materials 0.000 claims description 38
- 238000005468 ion implantation Methods 0.000 claims description 30
- 239000013077 target material Substances 0.000 claims description 26
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 20
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 16
- 229910052757 nitrogen Inorganic materials 0.000 claims description 16
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- 238000000151 deposition Methods 0.000 claims description 14
- 230000008021 deposition Effects 0.000 claims description 14
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- 238000002513 implantation Methods 0.000 claims description 12
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- 238000001816 cooling Methods 0.000 claims description 10
- 238000000605 extraction Methods 0.000 claims description 10
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- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 10
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- 238000007605 air drying Methods 0.000 claims description 5
- 238000004140 cleaning Methods 0.000 claims description 5
- 238000001035 drying Methods 0.000 claims description 5
- QJGQUHMNIGDVPM-UHFFFAOYSA-N nitrogen(.) Chemical compound [N] QJGQUHMNIGDVPM-UHFFFAOYSA-N 0.000 claims description 5
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- 238000002791 soaking Methods 0.000 claims description 2
- 150000002500 ions Chemical class 0.000 abstract description 9
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- 125000004433 nitrogen atom Chemical group N* 0.000 abstract 1
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- 239000011248 coating agent Substances 0.000 description 7
- -1 microcracks Substances 0.000 description 7
- 238000001764 infiltration Methods 0.000 description 5
- 238000011160 research Methods 0.000 description 5
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 4
- 230000006872 improvement Effects 0.000 description 4
- 239000000758 substrate Substances 0.000 description 4
- 229910001018 Cast iron Inorganic materials 0.000 description 3
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 3
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- 238000010849 ion bombardment Methods 0.000 description 2
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- 229910052742 iron Inorganic materials 0.000 description 2
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- 239000002184 metal Substances 0.000 description 2
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- 239000004202 carbamide Substances 0.000 description 1
- 238000005256 carbonitriding Methods 0.000 description 1
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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
- 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
- C23C14/48—Ion implantation
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/24—After-treatment of workpieces or articles
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F5/00—Manufacture of workpieces or articles from metallic powder characterised by the special shape of the product
- B22F5/08—Manufacture 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
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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
- 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
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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
- 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
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/24—After-treatment of workpieces or articles
- B22F2003/241—Chemical after-treatment on the surface
- B22F2003/242—Coating
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Abstract
The invention discloses a gradient ceramic wear-resistant alloy layer with a Ti/CrN composite structure and a preparation method thereof. The preparation method comprises the following steps: (1) injecting N strengthening layers into the surface of the powder metallurgy gear; (2) and preparing a Ti-Cr alloy layer on the surface of the N strengthening layer by using a double-glow plasma alloying method. The nitrogen atoms are easy to interact with alloy elements, and the formed nitride can improve the wear resistance. In the plasma alloying process, the sputtered Ti and Cr ions react with N injected by the ions to form a gradient ceramic wear-resistant alloy layer with a Ti/CrN composite structure. Compared with other methods for improving the wear resistance of the powder metallurgy gear, the method has the advantages that the two technical advantages are maximized, the wear resistance of the powder metallurgy gear is greatly improved, and the service life of the gear is prolonged.
Description
Technical Field
The invention belongs to the technical field of material science, and particularly relates to a gradient ceramic wear-resistant alloy layer with a Ti/CrN composite structure on the surface of a powder metallurgy gear and a preparation process thereof.
Background
For the gear, the problems of casting component segregation, long time of heat treatment processing and high energy consumption can be solved by powder metallurgy, so that the gear has more excellent overall performance and economic performance, and the manufacturing cost of the gear can be effectively reduced. But the stress condition of the gear is more complex during transmission, and the motion forms are also various, so the damage forms of the gear are also various. In general, gear damage is mainly in the form of tooth breakage, destructive gluing and destructive pitting. In order to prolong the service life of the gear, the gear can bear various types of damage, and the wear resistance of the surface of the powder metallurgy gear needs to be improved.
According to the current research, two main ways for improving the wear resistance of the powder metallurgy gear are provided, namely integral alloying. The traditional processing technology usually adopts the mode, but the integral alloying technology has high cost and great pollution; and secondly, a modified layer is formed on the surface of the iron-based gear through an advanced surface modification technology, so that the wear resistance of the gear is improved. Wear usually starts from the surface of the material, so that it is a more common method to improve the wear resistance of gears by surface modification. These surface modification techniques mainly include carburizing, nitriding, carbonitriding, thermal spraying, ion implantation, vacuum ion plating, and the like. The coating prepared by the thermal spraying process is mechanically combined with the gear, the bonding strength is low, the problems of pores, microcracks, coating peeling and the like are easy to occur in the using process, and the bonding strength of the coating and the gear is reduced; the ion implantation process may implant ions of the wear resistance enhancing element into the gear in a vacuum system to form an implanted layer with enhanced wear resistance. But the thickness of the ion implantation layer is not high, and only linear implantation can be carried out, so that the wear resistance of the gear cannot be comprehensively improved; the surface alloy layer prepared by the double glow plasma alloying technology comprises an alloy layer and a diffusion layer, the components and the performance are distributed along with the depth gradient, the combination with the matrix is firm, the alloy layer has compact structure and no defects of gaps, cracks and the like, and the working efficiency is high.
The double-layer glow plasma surface metallurgy technology (hereinafter referred to as "double glow technology") is a new metal surface alloying technology independently invented by Chinese scholars on the basis of ion nitriding. The working principle is that in a vacuum container, a furnace body is grounded as an anode, two cathodes are respectively arranged, one is used for placing a workpiece, the other is used for placing a source electrode for providing alloy elements, and argon with certain air pressure is introduced. Two sets of independent power supplies are arranged in the furnace, and glow is respectively generated between the anode and the source electrode and between the anode and the workpiece electrode after voltage is loaded, namely double-layer glow. Argon ions generated by glow discharge on the source bombard the target material and sputter target material electrode elements; sputtering of the workpiece pole heats the workpiece. The source voltage is set to be lower than the workpiece potential while the source power density is made higher than the workpiece power density. Thus, the amount of source sputtering will be much greater than the amount of reverse sputtering of the cathode. At high temperature, the alloy elements in the target material are deposited and diffused on the surface of the workpiece to form an alloy layer. The alloy layer is formed by diffusion of the alloying element into the base material and interaction with the base element.
The 'hot working process' published in 1997 'influence of density on the wear resistance of a multi-element co-infiltration layer of an iron-based powder metallurgy material' discloses a method for improving the wear resistance of the powder metallurgy material by a multi-element co-infiltration process taking methanol and urea as main infiltration agents; in the 3 rd phase of optical machinery published in 1988, "research on improving the wear resistance of powder metallurgy materials by laser treatment", a method for improving the wear resistance of powder metallurgy materials by laser treatment is disclosed; the book "university of Jiangsu science and technology" published in 2009: in the 2 nd phase of 'the current research situation of gear surface modification technology' of volume 23 of the natural science edition, a method for coating Ni-W and Ni-CO alloy coatings on the tooth surface of an HT250 cast iron gear by vacuum ion plating is disclosed, and compared with the uncoated cast iron gear, the wear resistance of the cast iron gear can be improved by 4-6 times. In the book of 30 rd phase of the book of vacuum science and technology journal of the 2010, "research on vacuum tribology performance of 30CrMnSi material for an ion implantation space gear transmission pair" in volume 3, a method for improving the wear resistance of a gear by implanting Ti, C and N elements on the gear by adopting ion implantation is disclosed. However, the ion implantation technology has the disadvantages of insufficient depth and small thickness of the implanted layer, which also limits the application of the ion implantation technology in the surface strengthening technology of the gear. Shenyang institute of engineering academy of Shenyang, published 2013: the article "application research of gear wear protection technology of power station coal mill" in the No. 1 of volume 9 of the Natural science edition discloses a method for improving the wear resistance of gear surface by using thermal spraying technology. However, the coating prepared by the process is mechanically combined with the gear, the bonding strength is low, the problems of pores, microcracks, coating peeling and the like are easy to occur in the using process, and the bonding strength of the coating and the gear is reduced. A study on the improvement of the wear resistance of the gamma-TiAl-based alloy through biglow plasma Cr-Si co-infiltration in the No. 39 volume 3 of rare metals and hard alloys published in 2011 discloses a method for improving the wear resistance of a matrix by preparing a Cr-Si infiltration layer through a biglow plasma alloying technology.
Because the wear resistance of the powder metallurgy gear is difficult to meet the use requirement, a surface modification technology is needed to improve the wear resistance of the powder metallurgy gear. However, most of the currently published studies adopt a surface modification method to improve the wear resistance of the matrix, and the existing modification techniques have respective problems, such as: the single ion implantation method has the advantages that the implantation layer is thin, and the improvement of the wear resistance is limited, so that the service life of the implantation layer under the working condition is short; the temperature of the pure double-glow plasma alloying technology is high, which may cause gear deformation and influence the organization structure of the gear, so that the overall performance of the gear is reduced.
In order to meet the requirement of high wear resistance of the gear, two or more modification modes are required to be used in combination. But the single technology has limitations and its advantages are difficult to maximize. If the injection depth of ion injection is insufficient, the injection layer is thin, the improvement of the wear resistance of the gear is limited, and the service life of the injection layer is short under the working condition; the dual-glow plasma alloying technology can prepare an alloy layer with a certain thickness on the surface of the gear, and although the alloy layer can realize metallurgical bonding with a substrate, the simple dual-glow plasma alloying technology has higher temperature, which may cause the gear to deform, influence the organization structure of the gear and reduce the overall performance of the gear.
Disclosure of Invention
In view of the above problems, the present invention aims to provide a gradient ceramic wear-resistant alloy layer with a Ti/CrN composite structure and a preparation method thereof, wherein the alloy layer can greatly improve the wear-resistant performance of the surface of the powder metallurgy gear and prolong the service life of the powder metallurgy gear.
In order to achieve the purpose, the invention adopts the technical scheme that:
a preparation method of a gradient ceramic wear-resistant alloy layer with a Ti/CrN composite structure comprises the following steps:
(1) injecting N strengthening layers into the surface of the powder metallurgy gear;
(2) and preparing a Ti-Cr alloy layer on the surface of the N strengthening layer by using a double-glow plasma alloying method.
The step (1) comprises the following steps:
(1.1) carrying out ultrasonic treatment on the powder metallurgy gear, soaking the gear in alcohol or acetone, carrying out ultrasonic cleaning for 1-2 times, carrying out treatment for 20-30 min each time, and then drying;
(1.2) putting the powder metallurgy gear into a cavity of ion injection equipment, introducing argon, and carrying out pre-sputtering cleaning on the powder metallurgy gear cleaned by alcohol or acetone for 20-30 min;
(1.3) in a vacuum degree of less than 10-3Carrying out N ion implantation treatment under the Pa condition, wherein the implantation time is 0.5-1.5 hours;
(1.4) taking out the gear after furnace cooling, and storing at room temperature.
In the step (1.2), the pre-sputtering parameters are as follows: the voltage is 500-700V, and the beam density is 0.2-0.4 muA/cm2Argon plasma density of 1X 109～3×109cm-3。
In the step (1.3), the process parameters of the N ion implantation treatment are as follows: the purity of the nitrogen is 99.99 percent, the nitrogen ion injection voltage is 30-50 kV, and the beam density is 2-2.5 muA/cm2Nitrogen plasma density of 1X 109～3×109cm-3The implantation dose is 3X 1017～6×1017ions/cm2。
The step (2) comprises the following steps:
(2.1) polishing the Ti-Cr target material prepared by the powder metallurgy method step by using sand paper, immersing the Ti-Cr target material into alcohol or acetone for ultrasonic cleaning for 20-30 min, and placing the Ti-Cr target material into a double-glow device furnace after air drying;
(2.2) adjusting the inter-pole distance, namely, the distance between the lower surface of the Ti-Cr target and the upper surface of the gear is 18-20 mm, and closing a furnace cover, an air release valve and a vent valve;
(2.3) opening the mechanical pump, then opening the air extraction valve, and vacuumizing to 10 DEG-3Below Pa, closing the air extraction valve;
(2.4) opening an argon bottle, opening an argon valve, then opening a flowmeter, introducing argon, performing gas washing treatment, opening a vacuum valve and closing an argon flow valve when the air pressure of the device reaches 145-160 Pa, reducing the air pressure to 35-40 Pa, and repeating the gas washing steps for 3-5 times;
(2.5) adjusting the air pressure to 30-40 Pa;
(2.6) starting circulating water at the temperature of 40-50 ℃;
(2.7) turning on a workpiece electrode power supply, starting glow by utilizing a hollow cathode effect, gradually regulating the voltage of a source electrode to be 500-600V and the voltage of the workpiece electrode to be 300-450V after glow is stable, and bombarding the gear for more than 0.5 h;
(2.8) gradually adjusting the workpiece electrode voltage and the source electrode voltage until the source electrode voltage is 900-940V and the workpiece electrode voltage is 520-550V.
(2.9) preserving the heat for 2.5-3.5 hours;
(2.10) gradually and slowly reducing the voltage of the source electrode and the workpiece electrode to be 0, wherein the time is more than 0.5h for avoiding stress concentration;
(2.11) closing an argon valve, a vacuum valve, a mechanical pump, a power switch and a circulating water switch;
(2.12) cooling for more than 2 hours, and taking out the gear.
The Ti-Cr target material comprises 60-70 wt% of Ti and 30-40 wt% of Cr.
The gradient ceramic wear-resistant alloy layer with the Ti/CrN composite structure prepared by the method sequentially comprises a Ti-Cr deposition layer, a Ti/CrN gradient ceramic layer and an N strengthening layer from top to bottom.
The thickness of the Ti-Cr deposition layer is 15-20 mu m, and the total thickness of the Ti/CrN gradient ceramic layer and the N strengthening layer is 3-6 mu m.
The Ti and Cr contents of the Ti/CrN gradient layer are reduced in a gradient manner from the outside to the inside, and the N content is increased in a gradient manner from the outside to the inside.
Has the advantages that: the invention combines ion implantation and double glow plasma alloying technology to prepare a ceramic wear-resistant alloy layer with a Ti/CrN composite structure. Firstly, injecting N into the surface of the gear, and secondly, preparing the gradient ceramic wear-resistant alloy layer by using a dual-glow plasma alloying technology. The method can greatly improve the wear resistance of the surface of the powder metallurgy gear and prolong the service life of the powder metallurgy gear. Has the following advantages:
1. after N is implanted into the ions, an injection layer is formed on the surface of the gear, surface grains are refined, and the wear resistance is improved to a certain extent.
The Ti-Cr layer is an ion bombardment sputtering deposition layer, and the layer has compact structure and no pores or cracks. The N injected by the ions reacts with the sputtered Ti and Cr after diffusion to form a Ti/CrN ceramic layer, the components and the performance of the Ti/CrN ceramic layer are distributed along with the depth gradient, the Ti/CrN ceramic layer is metallurgically bonded with the gear, the bonding strength is high, and the Ti/CrN ceramic layer is not easy to fall off.
3. The effects of each area of the gradient ceramic wear-resistant alloy layer with the Ti/CrN composite structure are as follows: (1) the Ti-Cr deposition layer plays a role in lubricating the soft film in friction, so that the friction coefficient is reduced, and the wear resistance is improved; (2) the Ti/CrN ceramic layer has higher hardness, so that the wear resistance of the composite structure alloy layer is further improved; (3) the ion implantation of the N strengthening layer enables the ceramic layer and the substrate to realize interface-free transition connection, and meanwhile, the hardness of the N strengthening layer is higher than that of the substrate, so that the abrasion resistance of the substrate is improved. In conclusion, the gradient wear-resistant alloy layer with the Ti/CrN composite structure greatly improves the wear resistance and service life of the powder metallurgy gear.
4. The single techniques for improving wear resistance have respective problems: the single ion implantation method has the advantages that the implantation layer is thin, and the improvement of the wear resistance is limited, so that the service life of the implantation layer under the working condition is short; the temperature of the pure double-glow plasma alloying technology is high, which may cause gear deformation and influence the organization structure of the gear, so that the overall performance of the gear is reduced. The invention combines ion implantation and double glow plasma alloying technology to prepare a gradient ceramic wear-resistant alloy layer with a Ti/CrN composite structure. The invention overcomes the problems existing in a single technology, realizes maximization of the advantages of the two technologies, greatly improves the wear resistance of the powder metallurgy gear, and greatly prolongs the service life of the gear.
Drawings
FIG. 1 is a schematic view of a gradient wear-resistant alloy layer with a Ti/CrN composite structure.
Fig. 2 is an SEM image of the composite structure gradient wear-resistant alloy layer prepared in example 1.
Detailed Description
The present invention will be described in further detail with reference to examples. But it is well within the ability of those skilled in the art to reasonably generalize and deduce the same based on the values set forth in the detailed description.
The purity of argon, the purity of Ti and the purity of Cr used in the following were 99.99%, 99.99% and 99.99%, respectively. The ion implantation equipment used in the following examples is LZX-700 high-energy metal ion implantation equipment (MEVVA ion source) manufactured by beijing tai kno ltd, and the dual-glow plasma alloying experiment was self-developed and entrusted to dual-glow plasma surface metallurgy equipment manufactured by shenyang scientific instrument development center ltd of the chinese academy of sciences.
Example 1
(1) Ion implantation of N:
(1.1) carrying out ultrasonic treatment on the powder metallurgy gear, immersing the gear in alcohol, carrying out ultrasonic cleaning twice, carrying out treatment for 30min each time, removing impurities on the surface, and then drying;
(1.2) putting the gear into a cavity of ion implantation equipment, introducing argon, and carrying out pre-sputtering cleaning on the powder metallurgy gear cleaned by alcohol for 30min, wherein the set parameters are as follows: the voltage is 500V, and the beam current density is 0.2 muA/cm2Argon plasma density of 1X 109cm-3；
(1.3) starting N ion implantation treatment, and setting the process parameters as follows: vacuum degree lower than 10-3Pa, nitrogen purity of 99.99%, nitrogen ion injection voltage of 35kV, and beam density of 2 μ A/cm2Nitrogen plasma density of 1X 109cm-3The implantation dose is 3X 1017ions/cm2The injection time is 1 hour;
(1.4) taking out the gear after furnace cooling, and storing at room temperature.
(2) Preparing a Ti-Cr alloy layer by using a dual-glow plasma alloying technology:
(2.1) polishing the Ti-Cr target material prepared by powder metallurgy step by using sand paper, immersing the Ti-Cr target material into alcohol for ultrasonic cleaning for 30min to ensure the surface purity, and placing the Ti-Cr target material into a double-glow device furnace after air drying;
(2.2) adjusting the inter-pole distance, namely, the distance between the lower surface of the Ti-Cr target and the upper surface of the gear is 18mm, and closing the furnace cover, the air release valve and the vent valve;
(2.3) opening the mechanical pump, then opening the air extraction valve, and vacuumizing to 10 DEG-3The vacuum degree in the furnace is ensured below Pa, and the air extraction valve is closed;
and (2.4) opening an argon bottle, opening an argon valve, then opening a flowmeter, introducing argon, and carrying out gas washing treatment. When the air pressure of the device reaches 150Pa, opening a vacuum valve and closing an argon flow valve to reduce the air pressure to 40Pa, and repeating the air washing steps for three times;
(2.5) adjusting the air pressure to 40 Pa;
(2.6) starting circulating water at the temperature of 45 ℃;
(2.7) turning on a workpiece electrode power supply, starting glow by utilizing a hollow cathode effect, gradually regulating the voltage of a source electrode to be 500V and the voltage of the workpiece electrode to be 300V after glow is stable, and bombarding the gear for 0.5h to prevent the gear from being polluted or oxidized after ion implantation;
(2.8) gradually adjusting the workpiece electrode voltage and the source electrode voltage until the source electrode voltage is 900V and the workpiece electrode voltage is 520V; (2.9) preserving the heat for 2.5 hours;
(2.10) after the heat preservation is finished, gradually and slowly reducing the voltage of the source electrode and the workpiece electrode to be 0, wherein the time is more than 0.5h for avoiding stress concentration;
(2.11) closing an argon valve, a vacuum valve, a mechanical pump, a power switch and a circulating water switch;
(2.12) taking out the gear after cooling for 2 hours.
The mass fraction of Ti in the Ti-Cr target material is 60 wt%, and the mass fraction of Cr in the Ti-Cr target material is 40 wt%. The prepared wear-resistant alloy layer with the composite structure on the surface of the powder metallurgy gear is respectively a Ti-Cr deposition layer, a Ti/CrN gradient ceramic layer and an N strengthening layer from top to bottom. Wherein, the Ti and Cr contents in the Ti/CrN gradient ceramic layer are reduced in a gradient way from the surface to the inside, and the N content is increased in a gradient way from the surface to the inside. The thickness of the Ti-Cr deposition layer is about 15 μm, and the total thickness of the Ti/CrN gradient ceramic layer and the N strengthening layer is 4 μm.
The friction and wear test shows that the wear rate of the treated powder metallurgy gear is reduced by 68.4 percent compared with that of the untreated gear. FIG. 2 is an SEM image of the gradient wear-resistant alloy layer with a composite structure prepared in example 1, wherein the area I is a Ti-Cr deposition layer, and the Ti-Cr layer is an ion bombardment sputtering deposition layer, has compact structure and is free of holes and cracks; the II area is a gradient ceramic layer and an N strengthening layer, the components of the II area are distributed in a gradient manner, the II area is combined with the gear through metallurgical combination, the combination strength is high, and the II area is not easy to fall off.
Example 2
(1) Ion implantation of N:
(1.1) carrying out ultrasonic treatment on the powder metallurgy gear, immersing the gear in alcohol, carrying out ultrasonic cleaning twice, carrying out treatment for 20min each time, removing impurities on the surface, and then drying;
(1.2) putting the gear into a cavity of ion implantation equipment, introducing argon, and carrying out pre-sputtering cleaning on the powder metallurgy gear cleaned by alcohol for 20min, wherein the set parameters are as follows: the voltage is 600V, and the beam current density is 0.3 muA/cm2Argon plasma density of 2X 109cm-3；
(1.3) starting N ion implantation treatment, and setting the process parameters as follows: vacuum degree lower than 10-3Pa, nitrogen purity of 99.99%, nitrogen ion injection voltage of 45kV, and beam density of 2.2 μ A/cm2Nitrogen plasma density of 2X 109cm-3The implantation dose is 5 × 1017ions/cm2The injection time was 1.5 hours.
(1.4) taking out the gear after furnace cooling, and storing at room temperature.
(2) Preparing a Ti-Cr alloy layer by using a dual-glow plasma alloying technology:
(2.1) polishing the Ti-Cr target material prepared by powder metallurgy step by using sand paper, immersing the Ti-Cr target material into alcohol for ultrasonic cleaning for 30min to ensure the surface purity, and placing the Ti-Cr target material into a double-glow device furnace after air drying;
(2.2) adjusting the inter-pole distance, namely, the distance between the lower surface of the Ti-Cr target and the upper surface of the gear is 19mm, and closing the furnace cover, the air release valve and the vent valve;
(2.3) opening the mechanical pump, then opening the air extraction valve, and vacuumizing to 10 DEG-3The vacuum degree in the furnace is ensured below Pa, and the air extraction valve is closed;
(2.4) opening an argon bottle, opening an argon valve, then opening a flowmeter to introduce argon, performing gas washing treatment, opening a vacuum valve and closing an argon flow valve when the air pressure of the device reaches 150Pa, reducing the air pressure to 40Pa, and repeating the gas washing steps for three times;
(2.5) adjusting the air pressure to 40 Pa;
(2.6) starting circulating water at the temperature of 45 ℃;
(2.7) turning on a workpiece electrode power supply, starting glow by utilizing a hollow cathode effect, gradually regulating the source voltage to 550V and the workpiece electrode voltage to 400V after glow is stable, and bombarding the gear at a low temperature for 0.5h to prevent the gear from being polluted or oxidized after ion implantation;
(2.8) gradually adjusting the workpiece electrode voltage and the source electrode voltage until the source electrode voltage is 920V and the workpiece electrode voltage is 540V;
(2.9) preserving the heat for 3 hours;
(2.10) after the heat preservation is finished, gradually and slowly reducing the voltage of the source electrode and the workpiece electrode to be 0, wherein the time is more than 0.5h for avoiding stress concentration;
(2.11) closing an argon valve, a vacuum valve, a mechanical pump, a power switch and a circulating water switch;
(2.12) taking out the gear after cooling for 4 hours.
The mass fraction of Ti in the Ti-Cr target material is 60 wt%, and the mass fraction of Cr in the Ti-Cr target material is 40 wt%. The prepared wear-resistant alloy layer with the composite structure on the surface of the powder metallurgy gear is respectively a Ti-Cr deposition layer, a Ti/CrN gradient ceramic layer and an N strengthening layer from top to bottom. Wherein, the Ti and Cr contents in the Ti/CrN gradient ceramic layer are reduced in a gradient way from the surface to the inside, and the N content is increased in a gradient way from the surface to the inside. The thickness of the Ti-Cr deposition layer is about 17 μm and the total thickness of the Ti/CrN gradient ceramic layer and the N strengthening layer is 5 μm, as can be obtained by line scanning.
The friction and wear test shows that the wear rate of the treated powder metallurgy gear is reduced by 72.4 percent compared with that of the untreated gear.
Example 3
(1) Ion implantation of N:
(1.1) carrying out ultrasonic treatment on the powder metallurgy gear, immersing the gear in acetone, carrying out ultrasonic cleaning for 1 time, treating for 25min, removing impurities on the surface, and then drying;
(1.2) putting the gear into a cavity of ion implantation equipment, introducing argon, and carrying out pre-sputtering cleaning on the powder metallurgy gear cleaned by acetone for 25min, wherein the setting parameters are as follows: the voltage is 700V, and the beam current density is 0.4 muA/cm2Argon plasma density of 3X 109cm-3；
(1.3) starting N ion implantation treatment, and setting the process parameters as follows: vacuum degree lower than 10-3Pa, nitrogen purity of 99.99%, nitrogen ion injection voltage of 50kV, and beam density of 2.5 μ A/cm2Nitrogen plasma density of 3X 109cm-3The implantation dose is 6 x 1017ions/cm2The injection time is 1.5 hours;
(1.4) taking out the gear after furnace cooling, and storing at room temperature.
(2) Preparing a Ti-Cr alloy layer by using a dual-glow plasma alloying technology:
(2.1) polishing the Ti-Cr target material prepared by powder metallurgy step by using abrasive paper, immersing the Ti-Cr target material into alcohol for ultrasonic cleaning for 25min to ensure the surface purity, and placing the Ti-Cr target material into a double-glow device furnace after air drying;
(2.2) adjusting the inter-pole distance, namely, the distance between the lower surface of the Ti-Cr target and the upper surface of the gear is 20mm, and closing the furnace cover, the air release valve and the vent valve;
(2.3) opening the mechanical pump, then opening the air extraction valve, and vacuumizing to 10 DEG-3The vacuum degree in the furnace is ensured below Pa, and the air extraction valve is closed;
(2.4) opening an argon bottle, opening an argon valve, then opening a flowmeter, introducing argon, performing gas washing treatment, opening a vacuum valve and closing an argon flow valve when the air pressure of the device reaches 150Pa, reducing the air pressure to 35Pa, and repeating the gas washing step for 5 times;
(2.5) adjusting the air pressure to 35 Pa;
(2.6) starting circulating water at 40 ℃;
(2.7) turning on a workpiece electrode power supply, starting glow by utilizing a hollow cathode effect, gradually regulating the voltage of a source electrode to 600V and the voltage of the workpiece electrode to 450V after glow is stable, and bombarding the gear at a low temperature for 1h to prevent the gear from being polluted or oxidized after ion implantation;
(2.8) gradually adjusting the workpiece electrode voltage and the source electrode voltage until the source electrode voltage is 940V and the workpiece electrode voltage is 550V;
(2.9) preserving the heat for 3.5 hours;
(2.10) after the heat preservation is finished, gradually and slowly reducing the voltage of the source electrode and the workpiece electrode to be 0, wherein the time is more than 0.5h for avoiding stress concentration;
(2.11) closing an argon valve, a vacuum valve, a mechanical pump, a power switch and a circulating water switch;
(2.12) taking out the gear after cooling for 5 hours.
The mass fraction of Ti in the Ti-Cr target material is 70wt%, and the mass fraction of Cr in the Ti-Cr target material is 30 wt%. The prepared wear-resistant alloy layer with the composite structure on the surface of the powder metallurgy gear is respectively a Ti-Cr deposition layer, a Ti/CrN gradient ceramic layer and an N strengthening layer from top to bottom. Wherein, the Ti and Cr contents in the Ti/CrN gradient ceramic layer are reduced in a gradient way from the surface to the inside, and the N content is increased in a gradient way from the surface to the inside. The thickness of the Ti-Cr deposition layer is about 19 μm and the total thickness of the Ti/CrN gradient ceramic layer and the N strengthening layer is 6 μm, as can be obtained by line scanning.
The friction and wear test shows that the wear rate of the treated powder metallurgy gear is reduced by 73.2 percent compared with that of the untreated gear.
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and decorations can be made without departing from the principle of the present invention, and these modifications and decorations should also be regarded as the protection scope of the present invention.
Claims (7)
1. A preparation method of a gradient ceramic wear-resistant alloy layer with a Ti/CrN composite structure is characterized by comprising the following steps: comprises the following steps:
(1) injecting N strengthening layers into the surface of the powder metallurgy gear; comprises the following steps:
(1.1) carrying out ultrasonic treatment on the powder metallurgy gear, soaking the gear in alcohol or acetone, carrying out ultrasonic cleaning for 1 ~ 2 times, carrying out treatment for 20 ~ 30min each time, and then drying;
(1.2) putting the powder metallurgy gear into a cavity of ion injection equipment, introducing argon, and carrying out pre-sputtering cleaning on the powder metallurgy gear cleaned by alcohol or acetone for 20 ~ 30 min;
(1.3) in a vacuum degree of less than 10-3Carrying out N ion implantation treatment under the Pa condition, wherein the implantation time is 0.5 ~ 1.5.5 hours;
(1.4) taking out the gear after furnace cooling, and storing at room temperature;
(2) preparing a Ti-Cr alloy layer on the surface of the N strengthening layer by using a double-glow plasma alloying method; comprises the following steps:
(2.1) polishing the Ti-Cr target material prepared by the powder metallurgy method step by using sand paper, immersing the Ti-Cr target material into alcohol or acetone for ultrasonic cleaning for 20 ~ 30min, air-drying and placing the Ti-Cr target material into a double-glow device furnace;
(2.2) adjusting the inter-pole distance, namely, the distance between the lower surface of the Ti-Cr target and the upper surface of the gear is 18 ~ 20mm, and closing the furnace cover, the air release valve and the vent valve;
(2.3) opening the mechanical pump, then opening the air extraction valve, and vacuumizing to 10 DEG-3Below Pa, closing the air extraction valve;
(2.4) opening an argon bottle, opening an argon valve, then opening a flowmeter to introduce argon, performing gas washing treatment, opening a vacuum valve and closing an argon flow valve when the air pressure of the device reaches 145 ~ 160Pa, reducing the air pressure to 35 ~ 40Pa, and repeating the gas washing step for 3 ~ 5 times;
(2.5) adjusting the air pressure to the working air pressure of 30 ~ 40 Pa;
(2.6) starting circulating water at 40 ~ 50 ℃ and 50 ℃;
(2.7) turning on a workpiece electrode power supply, starting glow by utilizing a hollow cathode effect, gradually regulating the source voltage to 500 ~ 600V and the workpiece electrode voltage to 300 ~ 450V after glow is stable, and bombarding the gear for more than 0.5 h;
(2.8) gradually adjusting the workpiece voltage and the source voltage until the source voltage is 900 ~ 940V and the workpiece voltage is 520 ~ 550V;
(2.9) keeping the temperature for 2.5 ~ 3.5.5 hours;
(2.10) gradually and slowly reducing the voltage of the source electrode and the workpiece electrode to be 0, wherein the time is more than 0.5h for avoiding stress concentration;
(2.11) closing an argon valve, a vacuum valve, a mechanical pump, a power switch and a circulating water switch;
(2.12) cooling for more than 2 hours, and taking out the gear.
2. The method for preparing the Ti/CrN composite structure gradient ceramic wear-resistant alloy layer according to claim 1, wherein in the step (1.2), the pre-sputtering parameters comprise that the voltage is 500-700V, and the beam current density is 0.2 ~ 0.4.4 muA/cm2Argon plasma density of 1X 109～3×109cm-3。
3. The method for preparing a gradient ceramic wear-resistant alloy layer of a Ti/CrN composite structure according to claim 1, wherein: in the step (1.3), the process parameters of the N ion implantation treatment are as follows: the purity of the nitrogen is 99.99 percent, the nitrogen ion injection voltage is 30-50 kV, and the beam density is 2-2.5 muA/cm2Nitrogen plasma density of 1X 109～3×109cm-3The implantation dose is 3X 1017~6×1017ions/cm2。
4. The method for preparing a Ti/CrN composite structure gradient ceramic wear-resistant alloy layer according to claim 1, wherein the Ti-Cr target material comprises Ti 60wt 60 ~ 70wt% and Cr 30 ~ 40 wt%.
5. A gradient ceramic wear-resistant alloy layer with a Ti/CrN composite structure prepared by the method of claim 1 ~ 4 is characterized by sequentially comprising a Ti-Cr deposition layer, a Ti/CrN gradient ceramic layer and an N strengthening layer from top to bottom.
6. The Ti/CrN composite structure gradient ceramic wear-resistant alloy layer as set forth in claim 5, wherein the Ti-Cr deposition layer has a thickness of 15 ~ 20 μm, and the Ti/CrN gradient ceramic layer and the N strengthening layer have a total thickness of 3 ~ 6 μm.
7. The gradient ceramic wear-resistant alloy layer of Ti/CrN composite structure according to claim 5, characterized in that: the Ti and Cr contents of the Ti/CrN gradient layer are reduced in a gradient manner from the outside to the inside, and the N content is increased in a gradient manner from the outside to the inside.
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