CN110666177A - Multilayer nanocrystalline composite structure NiCrAlBNb-based bearing retainer material and preparation method thereof - Google Patents

Multilayer nanocrystalline composite structure NiCrAlBNb-based bearing retainer material and preparation method thereof Download PDF

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CN110666177A
CN110666177A CN201910997700.5A CN201910997700A CN110666177A CN 110666177 A CN110666177 A CN 110666177A CN 201910997700 A CN201910997700 A CN 201910997700A CN 110666177 A CN110666177 A CN 110666177A
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nicralbnb
layer
friction film
bearing retainer
multilayer
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马洪儒
曹增志
曹帅涛
卞会涛
王连富
李爱虎
李淦鑫
张文帆
王秋菊
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Anyang Institute of Technology
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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
    • B22F7/00—Manufacture of composite layers, workpieces, or articles, comprising metallic powder, by sintering the powder, with or without compacting wherein at least one part is obtained by sintering or compression
    • B22F7/02—Manufacture of composite layers, workpieces, or articles, comprising metallic powder, by sintering the powder, with or without compacting wherein at least one part is obtained by sintering or compression of composite layers
    • 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
    • B22F3/12—Both compacting and sintering
    • B22F3/14—Both compacting and sintering simultaneously
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C19/00—Alloys based on nickel or cobalt
    • C22C19/03—Alloys based on nickel or cobalt based on nickel
    • C22C19/05—Alloys based on nickel or cobalt based on nickel with chromium
    • C22C19/058—Alloys based on nickel or cobalt based on nickel with chromium without Mo and W
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C30/00—Alloys containing less than 50% by weight of each constituent
    • C22C30/04—Alloys containing less than 50% by weight of each constituent containing tin or lead
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C47/00—Making alloys containing metallic or non-metallic fibres or filaments
    • C22C47/14—Making alloys containing metallic or non-metallic fibres or filaments by powder metallurgy, i.e. by processing mixtures of metal powder and fibres or filaments
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C49/00—Alloys containing metallic or non-metallic fibres or filaments
    • C22C49/02—Alloys containing metallic or non-metallic fibres or filaments characterised by the matrix material
    • C22C49/08—Iron group metals
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C49/00—Alloys containing metallic or non-metallic fibres or filaments
    • C22C49/14—Alloys containing metallic or non-metallic fibres or filaments characterised by the fibres or filaments

Abstract

The invention relates to a multilayer nanocrystalline composite structure NiCrAlBNb-based bearing retainer material and a preparation method thereof. The main components of the bearing retainer comprise a NiCrAlBNb matrix, soft alloy PbSnAgBiSb and a multi-component composite regulating agent. The NiCrAlBNb-based bearing retainer processing flow is preparation of a multi-element plate crystal, design calculation of materials of all layers, vibration mixing, hot press molding and sample processing, compounding of a multi-layer structure, and rolling treatment of the materials. Compared with the evenly distributed bearing retainer material, the NiCrAlBNb-based multilayer nanocrystalline composite structure material greatly saves the material usage amount on the premise of meeting the performance requirement of the bearing retainer material, and meanwhile, the multilayer nanocrystalline composite structure can enable the bearing retainer to replace oil and grease to realize a good lubricating effect under the working conditions of high temperature, high pressure and the like, and has the advantages of environmental protection, high use precision, long service life and the like.

Description

Multilayer nanocrystalline composite structure NiCrAlBNb-based bearing retainer material and preparation method thereof
Technical Field
The invention relates to a multilayer nanocrystalline composite structure NiCrAlBNb-based bearing retainer material and a preparation method thereof, belongs to an innovative research in the technical field of bearings, retainers and the like, and can replace a traditional bearing retainer to realize good lubricating performance under extreme working conditions of high temperature, high pressure, high speed, high vacuum and the like.
Technical Field
The alloy material used as the bearing retainer at present is required to have good thermal conductivity, excellent wear resistance, lower friction coefficient, low density, high strength and high toughness, excellent elasticity and rigidity, linear expansion coefficient similar to that of a rolling body and the like. The cage is also subjected to friction by chemical agents, such as lubricants, lubricant additives, organic solvents and coolants [ Wangziking, Limited design of Rolling bearings, Haerbin university Press, 2013.12 ]. At present, the bearing retainer material mainly comprises a steel retainer material, a non-ferrous metal retainer material, a non-metallic retainer material (a kindred steel, a Lixing forest, a Wangyong and the like), a common sense 2 nd edition of rolling bearings is used, and a mechanical industry publisher, 2015.03, and a very thin lubricating oil film is required to be arranged between a bearing rolling body and the retainer in the working process of the rolling bearing retainer material to achieve a good lubricating effect. However, in actual work, working conditions such as temperature and load, impact, vibration and the like are main reasons for causing the damage of a lubricating oil film of the bearing retainer, a light person affects the direct tribological performance between the rolling body and the retainer, the retainer can be burned and broken in a serious condition, and even the lubricating bearing can be failed.
Disclosure of Invention
Aiming at the technical defects, the invention provides a multilayer nanocrystalline composite structure NiCrAlBNb-based bearing retainer material and a preparation method thereof, and on the premise of meeting good heat conductivity, excellent wear resistance, low friction, small density and the like, the multilayer nanocrystalline composite structure NiCrAlBNb-based bearing retainer material can realize the lubrication effect which can not be achieved by oil and grease under the working conditions of high temperature, high pressure and the like, has potential scientific value for improving the use precision and service life of the retainer, and provides research methods and technical guidance for the design and preparation of bearing retainers such as aerospace and high-end manufacturing equipment.
The invention relates to a multilayer nanocrystalline composite structure NiCrAlBNb-based bearing retainer material and a preparation method thereof, aiming at solving the problems of burning and fracture of a bearing retainer under the condition that oil and grease can not realize lubrication, the adopted technical scheme can be described as follows:
a multi-layer nanocrystalline composite structure NiCrAlBNb-based bearing retainer material is characterized in that a substrate NiCrAlBNb, soft alloy PbSnAgBiSb and a multi-element composite regulating agent are used as raw materials, and the multi-layer nanocrystalline composite structure NiCrAlBNb-based bearing retainer material is prepared through the process flows of layer-by-layer design, layer-by-layer proportioning, layer-by-layer preparation, overlapping molding and the like.
The method comprises the following steps:
a multi-layer nano-crystal composite NiCrAlBNb-based bearing retainer material and a preparation method thereof are disclosed, wherein a substrate NiCrAlBNb, a soft alloy PbSnAgBiSb and a multi-element composite regulating agent are used as raw materials, and the multi-layer nano-crystal composite material taking the NiCrAlBNb as the bearing retainer substrate is prepared through the process flows of layer-by-layer design, layer-by-layer proportioning, layer-by-layer preparation, overlapping molding and the like.
The multi-layer nanocrystalline composite NiCrAlBNb-based bearing retainer material in the step 1) comprises Ni, Cr, Al, B, Nb, Si, Co and Y, wherein the mass ratio of the elements is (70-80): 5-16): 4-7): 3-6): 2-4): 0.32-0.46): 0.2-0.4): 0.2-0.5; the mass ratio of each element of the soft alloy PbSnAgBiSb is (30-38): (23-27): (23-28): (15-18): (7-10).
The multilayer nanocrystalline composite NiCrAlBNb-based bearing retainer material in the step 1) consists of a metal substrate, a friction film transition layer, a friction film supporting layer and a friction film contact layer, and the thickness ratio of each corresponding layer is (45-65): (15-23): (10-20): (5-12).
The preparation method of the multilayer nanocrystalline composite structure NiCrAlBNb-based bearing retainer material in the step 3) comprises the steps that the components of a metal matrix, a friction film transition layer, a friction film supporting layer and a friction film contact layer are different, and the metal matrix is NiCrAlBNb-based high-temperature alloy; the friction film transition layer comprises NiCrAlBNb alloy, soft alloy PbSnAgBiSb and a multi-element composite regulating agent in a mass ratio of (40-55) to (15-20) to (25-45); the friction film supporting layer comprises a NiCrAlBNb matrix, soft alloy PbSnAgBiSb and a multi-element composite regulating agent, and the mass ratio of the soft alloy PbSnAgBiSb to the multi-element composite regulating agent is (10-15) to (10-13) to (72-80); the friction film contact layer comprises NiCrAlBNb alloy, soft alloy PbSnAgBiSb and a multi-element composite regulating agent in a mass ratio of (3-5) to (40-45) to (50-57).
The multilayer nanocrystalline composite structure NiCrAlBNb-based bearing retainer material and the preparation method thereof in the step 4), wherein the multiple composite regulating agent has different proportions in the components of the metal substrate, the friction film transition layer, the friction film supporting layer and the friction film contact layer, and the friction film transition layer comprises 5-10% of ceramic fiber, 11-15% of carbon fiber, 2.5-5.5% of glass fiber, 16-25% of nano white corundum, 11-15% of titanium carbide, 13-16% of tantalum carbide, 2-3.1% of fullerene, 2-2.5% of graphene, 3-5% of tungsten disulfide and 16-25% of multilayer platy crystal; the friction film supporting layer comprises 6-12% of ceramic fiber, 10-17% of carbon fiber, 4.5-8% of glass fiber, 11-15% of nano white corundum, 8.5-12% of titanium carbide, 14.5-17% of tantalum carbide, 1-1.6% of fullerene, 1-1.3% of graphene, 1.7-2.5% of tungsten disulfide and 22-33% of multilayer platy crystal; the friction film contact layer comprises 2.5-9% of ceramic fiber, 5-8.2% of carbon fiber, 2.5-5% of glass fiber, 10.5-17% of nano white corundum, 12-20% of titanium carbide, 17-24% of tantalum carbide, 3-3.6% of fullerene, 3.6-6% of graphene, 4.5-7.5% of tungsten disulfide and 21.1-26% of multilayer platy crystal.
The multilayer nanocrystalline composite structure NiCrAlBNb-based bearing retainer material and the preparation method thereof in the step 5), wherein the preparation process of the multilayer plate-shaped crystal material MoSiCrO comprises the steps of weighing ammonium molybdate, silicon powder and cadmium powder respectively according to the molar ratio of (3-4) to (2-3) to (1-2), grinding and mixing the powder materials such as ammonium molybdate and the like to obtain a plate-shaped crystal original ingredient which is uniformly mixed and has the average particle size of 40-45 mu m; and then sintering in a vacuum atmosphere furnace at the sintering temperature of 400-470 ℃, the heat preservation time of 5.5-6.5h and the protective gas of argon, wherein the oxygen amount is introduced in the sintering process of 75-125ml/min, and the multilayer platy crystal MoSiCrO is obtained.
The multilayer nanocrystalline composite structure NiCrAlBNb-based bearing retainer material and the preparation method thereof in the step 1) are prepared by processes of multielement plate crystal preparation, material design calculation of each layer, vibration mixing, hot press molding, sample processing, multilayer structure stacking firing, rolling and the like, and the multilayer composite structure NiCrAlBNb-based bearing retainer material is obtained.
The multilayer nanocrystalline composite NiCrAlBNb-based bearing retainer material and the preparation method thereof in the step 7), wherein each layer of material is subjected to hot press molding, uniformly mixed powder of each layer is respectively filled into a hot press molding die according to the component ratio of the metal substrate, the friction film transition layer, the friction film supporting layer and the friction film contact layer, and a composite metal sheet with the diameter of 18-28mm is obtained after sample processing.
The multilayer nanocrystalline composite structure NiCrAlBNb-based bearing retainer material and the preparation method thereof in the step 7) have the process flow of the multilayer composite structure, wherein the layers of the thin sheets prepared in the step 8 are sequentially arranged in a graphite mold with the diameter of 20-30mm, and the discharge plasma sintering process is arranged to prepare the multilayer structure NiCrAlBNb-based bearing retainer material.
The rolling treatment process comprises the step of repeatedly acting a ceramic-based rolling element on a friction film contact layer to form a nanocrystalline friction film, wherein the applied pressure is 5-10MPa, the linear velocity is 2-3m/s, and the temperature is 100oC, the action time is 30-50 min.
Compared with the prior art, the invention has the beneficial effects that:
1. the multilayer nanocrystalline composite structure NiCrAlBNb-based bearing retainer material can realize good frictional wear performance under the working conditions of high temperature, high pressure, high speed, high vacuum and the like, can achieve the lubrication effect which can not be realized by oil and grease, and has the advantages of environmental protection, long service life, high operation precision and the like;
2. the soft alloy PbSnAgBiSb and the multi-element composite material cooperate for lubrication, so that the tribological performance of the NiCrAlBNb-based bearing retainer is greatly improved, the requirements of the bearing retainer on the structural mechanical performance are met, and the comprehensive mechanical performance of the soft alloy PbSnAgBiSb and the multi-element composite material is more superior than that of the traditional bearing retainer material;
3. according to the multi-layer nanocrystalline composite structure NiCrAlBNb-based bearing retainer material, a NiCrAlBNb substrate is used as a connecting material among layers, so that the compatibility, the bonding property and the like of each layer are greatly improved, and the multi-layer nanocrystalline composite structure NiCrAlBNb-based bearing retainer material is an effective way for solving the technical problems of high-temperature peeling, easy separation of each layer and the like of a common multi-layer structure material.
Drawings
FIG. 1 is a flow chart of a manufacturing process embodying the present invention.
FIG. 2 is an electron micrograph of a multilayer plate-like crystalline MoSiCrO powder prepared in example 1.
FIG. 3 is a friction coefficient curve of a self-lubricating composite material of a multi-layer nanocrystalline NiCrAlBNb-based bearing retainer prepared in examples 1, 2 and 3 of the invention.
FIG. 4 is a histogram of wear rate of a multi-layer nanocrystalline NiCrAlBNb-based self-lubricating composite material for a bearing cage prepared in examples 1, 2 and 3 of the present invention.
FIG. 5 shows the electron microscope morphology of the self-lubricating composite material friction film transition layer and the friction film support layer of the multi-layer nanocrystalline NiCrAlBNb-based bearing retainer in the combined state, which is prepared under the conditions of example 2.
FIG. 6 is an electron probe morphology of a friction wear surface of a multi-layer nanocrystalline NiCrAlBNb-based bearing cage self-lubricating composite material prepared under the conditions of example 2.
FIG. 7 is a field emission scanning electron microscope appearance of a friction wear surface of a self-lubricating composite material of a multi-layer nanocrystalline NiCrAlBNb-based bearing retainer prepared in embodiment 3 of the invention.
FIG. 8 is a gray scale image of a 3D micro-morphology of the self-lubricating composite material of the multi-layer nanocrystalline NiCrAlBNb-based bearing cage in the form of frictional wear, which is prepared in example 3.
FIG. 9 is a black-white image of the 3D micro-morphology of the self-lubricating composite material of the multi-layer nano-crystalline NiCrAlBNb-based bearing cage in the friction wear state, which is prepared in example 3.
Detailed Description
In order to better develop the present invention and verify it, the following examples are given to illustrate some of the main research contents of the present invention, but the present invention is not limited to the following examples.
The friction test conditions in the following examples were: the load is 10-20N, the rotating speed is 0.15-0.25m/s, and the time is 70 min.
Example 1
As shown in figure 1, the design and the preparation method of the self-lubricating composite material of the multi-layer nanocrystalline NiCrAlBNb-based bearing retainer mainly comprise the following steps:
1) weighing ammonium molybdate, silicon powder and cadmium powder according to a molar ratio of 3:2:1, and grinding and mixing the ammonium molybdate powder, the silicon powder and the cadmium powder to obtain a plate crystal original ingredient which is uniformly mixed and has an average particle size of 40 mu m; and then sintering in a vacuum atmosphere furnace, wherein the sintering temperature is 400 ℃, the heat preservation time is 5.5 hours, the protective gas is argon, and the oxygen amount is 75ml/min in the sintering process, so that the multilayer platy crystal MoSiCrO is obtained. FIG. 2 is an electron micrograph of a multilayer plate-like crystalline MoSiCrO powder prepared in example 1;
2) calculating and batching the multilayer platy crystal MoSiCrO obtained in the step 1) with ceramic fiber, carbon fiber, glass fiber, nano white corundum, titanium carbide, tantalum carbide, fullerene, graphene and tungsten disulfide, wherein the proportions of the components of each layer of the multi-component composite regulating agent are different. The multi-element composite regulating agent at the transition layer of the friction film mainly comprises 5% of ceramic fiber, 11.5% of carbon fiber, 2.5% of glass fiber, 25% of nano white corundum, 11% of titanium carbide, 13% of tantalum carbide, 2% of fullerene, 2% of graphene, 3% of tungsten disulfide and 25% of multilayer platy crystal; the multi-element composite regulating agent on the friction film support layer mainly comprises 6% of ceramic fiber, 17% of carbon fiber, 4.5% of glass fiber, 11% of nano white corundum, 8.5% of titanium carbide, 16.2% of tantalum carbide, 1.1% of fullerene, 1% of graphene, 1.7% of tungsten disulfide and 33% of multilayer platy crystal; the multi-element composite regulating agent on the contact layer of the friction film mainly comprises 2.5 percent of ceramic fiber, 5 percent of carbon fiber, 2.5 percent of glass fiber, 10.5 percent of nano white corundum, 20 percent of titanium carbide, 22.4 percent of tantalum carbide, 3 percent of fullerene, 3.6 percent of graphene, 4.5 percent of tungsten disulfide and 26 percent of multilayer platy crystal;
3) respectively placing the multi-layer multi-element composite regulation and control ingredients prepared in the step 1) into a pneumatic vacuum vibration material mixer for mixing, wherein an outer tank of the vibration material mixer is a quartz tank, and a polytetrafluoroethylene tank is arranged in the outer tank; argon flow is used as a mixed power source, and the flow rate of the argon power gas is 125m3The vibration force generated to the tank body is 13000N, the vibration frequency is 50Hz, the vibration time is 50min, and the vacuum degree of the tank body is 2.85 multiplied by 10-2Pa, obtaining the uniformly mixed multi-component composite regulating agent of each layer and storing the regulating agent in a classified manner;
4) weighing Ni, Cr, Al, B, Nb, Si, Co and Y powder according to the mass ratio of 70:5:4:3:2:0.32:0.2: 0.2; weighing Pb, Sn, Ag, Bi and Sb powder according to the mass ratio of 30:23:23:15: 7; respectively filling NiCrAlBNb powder and PbSnAgBiSb powder into a crucible containing alcohol solution by using vacuum mixing and drying equipmentHeating in vacuum environment, boiling alcohol and vacuum evaporation to realize uniform mixing and vacuum drying, and respectively obtaining the powder material with uniformly mixed NiCrAlBNb and PbSnAgBiSb. Vacuum degree of vacuum mixing and drying is 2.1 × 10-2Pa, heating temperature of 37oC, boiling for 25 min;
5) the multi-element composite regulating material obtained in the step 2) and NiCrAlBNb alloy and soft alloy PbSnAgBiSb have different components in each layer structure. The metal matrix is pure NiCrAlBNb-based alloy, and the friction film transition layer consists of NiCrAlBNb, soft alloy PbSnAgBiSb and a multi-element composite regulating agent in a mass ratio of 40:15: 25; the friction film supporting layer consists of NiCrAlBNb alloy, soft alloy PbSnAgBiSb and a multi-element composite regulating agent in a mass ratio of 10:10: 72; the friction film contact layer consists of NiCrAlBNb alloy, soft alloy PbSnAgBiSb and a multi-element composite regulating agent in a mass ratio of 3:40: 50;
6) mixing the powder of the NiCrAlBNb base layers and the like in the step 5) by adopting a pneumatic vacuum mixer, wherein the outer tank of the pneumatic vacuum vibration mixer is a quartz tank, and a polytetrafluoroethylene tank is arranged in the quartz tank; the pneumatic mixing parameters of each layer are different. The argon gas flow of the transition layer of the friction film is 115m3H, vibration force 4500N, vibration frequency 35Hz, vibration time 110min, tank vacuum degree 3.0 × 10-2Pa. The argon gas flow of the friction membrane supporting layer is 120m3H, the vibration force generated to the tank body is 7500N, the vibration frequency is 50Hz, the vibration time is 100min, and the vacuum degree of the tank body is 3.2 multiplied by 10-2Pa; the flow rate of argon gas in the contact layer of the friction film is 130m3H, generating vibration force of 5000N to the tank body, vibration frequency of 30Hz, vibration time of 25min, and vacuum degree of the tank body of 3.3 multiplied by 10- 2Pa；
7) And (3) respectively loading the uniformly mixed powder of each layer in the step 6) into a hot-pressing forming die to respectively obtain the thin sheet structure materials of each layer, such as the metal matrix, the friction film transition layer and the like. Performing hot-press molding on the transitional layer of the friction film under the pressure of 17MPa and the pressing temperature of 320 ℃, keeping the temperature and the pressure for 220min each time, deflating for 2s every 15min, and repeating the operation for 7 times; the pressure applied by the friction membrane supporting layer is 15MPa, the pressing temperature is 220 ℃, the heat preservation and pressure maintaining time is 120min each time, the air is released for 2s every 35min, and the operation is repeatedly carried out for 4 times; the pressure applied by the friction film contact layer is 20MPa, the pressing temperature is 150 ℃, the heat preservation and pressure maintaining time is 40min each time, the air is discharged for 2s every 10min, and the operation is repeatedly carried out for 3 times;
8) processing the pressed sheet obtained in the step 7) by using a sample, turning at a turning speed of 500r/min to obtain a metal sheet with each layer thickness and a section diameter of 18 mm; the rotating speed of the grinding process is 120r/min, the rotating speed of the polishing machine for cleaning peripheral burrs and flashes and the rotating speed of the electrostatic spraying process equipment is 550r/min, the temperature is 65 ℃, and finally the thin slice with the surface roughness of Ra1.6 and the diameter of 18mm is obtained;
9) and (3) sequentially loading the sheets with the diameter of 18mm in the step 8) into a graphite mould with the diameter of 20mm, and preparing the NiCrAlBNb-based bearing retainer with the multilayer structure by using a spark plasma sintering process. The sintering temperature of the discharge plasma is 1000 DEGoC. Sintering pressure of 29MPa, heat preservation time of 20min, protective gas of argon, heating rate of 100oC/min；
10) Rolling the multi-layer NiCrAlBNb-based bearing retainer obtained in the step 9, wherein the rolling process is to utilize a ceramic-based rolling body to repeatedly act on a friction film contact layer to form a nanocrystalline friction film, the applied pressure is 5MPa, the linear velocity is 2m/s, and the temperature is 100 DEGoC, acting for 30min to finally obtain the multilayer nanocrystalline NiCrAlBNb-based bearing retainer material;
FIG. 3 is a friction coefficient curve of a self-lubricating composite material of a multi-layer nanocrystalline NiCrAlBNb-based bearing retainer prepared in examples 1, 2 and 3 of the invention; FIG. 4 is a histogram of wear rate of a multi-layer nanocrystalline NiCrAlBNb-based self-lubricating composite material for a bearing cage prepared in examples 1, 2 and 3 of the present invention. As shown in FIGS. 3 and 4, the self-lubricating composite material of the multi-layer nano-crystalline NiCrAlBNb-based bearing retainer prepared in example 1 has a low friction coefficient of about 0.33 and a low wear rate of about 2.64X 10-6mm3in/Nm. This shows that the self-lubricating composite material of the multi-layer nano-crystalline NiCrAlBNb-based bearing retainer prepared in example 1 has excellent antifriction and antiwear performances.
Example 2
As shown in figure 1, the design and the preparation method of the self-lubricating composite material of the multi-layer nanocrystalline NiCrAlBNb-based bearing retainer mainly comprise the following steps:
1) weighing ammonium molybdate, silicon powder and cadmium powder according to a molar ratio of 4:3:2, and grinding and mixing the ammonium molybdate powder, the silicon powder and the cadmium powder to obtain a plate crystal original ingredient which is uniformly mixed and has an average particle size of 45 mu m; then sintering in a vacuum atmosphere furnace, wherein the sintering temperature is 470 ℃, the heat preservation time is 6.5h, the protective gas is argon, and the oxygen amount is 125ml/min in the sintering process to obtain multilayer platy crystal MoSiCrO;
2) calculating and batching the multilayer platy crystal MoSiCrO obtained in the step 1) with ceramic fiber, carbon fiber, glass fiber, nano white corundum, titanium carbide, tantalum carbide, fullerene, graphene and tungsten disulfide, wherein the proportions of the components of each layer of the multi-component composite regulating agent are different. The multi-element composite regulating agent at the transition layer of the friction film mainly comprises 10% of ceramic fiber, 12.3% of carbon fiber, 5.5% of glass fiber, 16% of nano white corundum, 15% of titanium carbide, 16% of tantalum carbide, 3.1% of fullerene, 2.5% of graphene, 3.6% of tungsten disulfide and 16% of multilayer platy crystal; the multi-element composite regulating agent on the friction film support layer mainly comprises 12% of ceramic fiber, 10% of carbon fiber, 8% of glass fiber, 13.6% of nano white corundum, 12% of titanium carbide, 17% of tantalum carbide, 1.6% of fullerene, 1.3% of graphene, 2.5% of tungsten disulfide and 22% of multilayer platy crystal; the multi-element composite regulating agent on the contact layer of the friction film mainly comprises 9% of ceramic fiber, 7.2% of carbon fiber, 3.4% of glass fiber, 10.4% of nano white corundum, 16% of titanium carbide, 20% of tantalum carbide, 3% of fullerene, 4.5% of graphene, 6.4% of tungsten disulfide and 23.1% of plate-shaped crystal;
3) respectively placing the multi-layer multi-element composite regulation and control ingredients prepared in the step 1) into a pneumatic vacuum vibration mixer for mixing, wherein an outer vibration mixing tank is a quartz tank, a polytetrafluoroethylene tank is arranged in the outer vibration mixing tank, argon flow is used as a mixed power source, and the flow of argon power gas is 125m3The vibration force generated to the tank body is 13000N, the vibration frequency is 50Hz, the vibration time is 50min, and the vacuum degree of the tank body is 2.85 multiplied by 10-2Pa, obtaining the uniformly mixed multi-component composite regulating agent of each layer and classifyingStoring;
4) weighing Ni, Cr, Al, B, Nb, Si, Co and Y powder according to the mass ratio of 80:16:7:6:4:0.46:0.4: 0.5; weighing Pb, Sn, Ag, Bi and Sb powder according to the mass ratio of 38:27:28:18: 10; and respectively filling NiCrAlBNb powder and PbSnAgBiSb powder into a crucible containing alcohol solution by using vacuum mixing and drying equipment, heating in a vacuum environment, and boiling and vacuum evaporating by using alcohol to realize uniform mixing and vacuum drying to respectively obtain NiCrAlBNb and PbSnAgBiSb uniformly-mixed powder. Vacuum degree of vacuum mixing and drying is 5.3X 10-2Pa, heating temperature of 55oC, boiling for 40 min;
5) the multi-element composite regulating material obtained in the step 2) is different from NiCrAlBNb-based alloy and PbSnAgBiSb soft alloy in components in each layer structure. The metal matrix is NiCrAlBNb alloy, and the friction film transition layer is composed of NiCrAlBNb alloy, soft alloy PbSnAgBiSb and multi-element composite regulating agent in a mass ratio of 55:20: 45; the friction film supporting layer consists of NiCrAlBNb alloy, soft alloy PbSnAgBiSb and a multi-element composite regulating agent in a mass ratio of 15:13: 80; the friction film contact layer consists of NiCrAlBNb alloy, soft alloy PbSnAgBiSb and a multi-element composite regulating agent in a mass ratio of 5:45: 57;
6) mixing the powder of the NiCrAlBNb base layers and the like in the step 5) by adopting a pneumatic vacuum mixer, wherein the outer tank of the pneumatic vacuum vibration mixer is a quartz tank, and a polytetrafluoroethylene tank is arranged in the quartz tank; the pneumatic mixing parameters of each layer structure are different. The flow rate of argon gas in the transition layer of the friction film is 125m3The vibration force is 6200N, the vibration frequency is 40Hz, the vibration time is 150min, and the vacuum degree of the tank body is 3.4 multiplied by 10-2Pa. The argon gas flow of the friction membrane supporting layer is 125m3H, the vibration force generated to the tank body is 8100N, the vibration frequency is 55Hz, the vibration time is 120min, and the vacuum degree of the tank body is 3.6 multiplied by 10-2Pa, the flow rate of argon gas in the contact layer of the friction film is 135m3H, generating 6000N vibration force to the tank body, 43Hz vibration frequency, 35min vibration time, and 3.5 × 10 vacuum degree-2Pa；
7) And (3) respectively loading the uniformly mixed powder of each layer in the step 6) into a hot-pressing forming die to respectively obtain the sheet structures of each layer, such as the metal matrix, the friction film transition layer and the like. Performing hot-press molding on the transitional layer of the friction film under the pressure of 19MPa and the pressing temperature of 420 ℃, keeping the temperature and the pressure for 250min each time, deflating for 3s every 20min, and repeating the operation for 9 times; performing hot-press molding on the friction membrane supporting layer, wherein the applied pressure is 17MPa, the pressing temperature is 320 ℃, the heat preservation and pressure maintaining time is 150min each time, the air is released for 3s every 55min, and the operation is repeatedly performed for 6 times; hot-press forming friction film contact layer under pressure of 25MPa at 200 deg.C, maintaining the temperature and pressure for 50min each time, discharging gas for 3s every 20min, and repeating for 5 times;
8) processing the sample of the metal sheet obtained in the step 7), turning at a turning speed of 500r/min to obtain a metal sheet with a thickness of each layer and a diameter of a cross section of 28 mm; the rotation speed of the grinding process is 155r/min, burrs and flashes around the polishing machine are cleaned, the rotation speed of electrostatic spraying process equipment is 650r/min, the subsequent treatment is carried out at the temperature of 85 ℃, and finally the metal composite sheet with the surface roughness of Ra1.6 and the diameter of 28mm is obtained;
9) and (3) sequentially putting the sheets with the diameter of 28mm in the step 8) into a graphite mould with the diameter of 30mm, and preparing the NiCrAlBNb-based bearing retainer with the multilayer structure by using a spark plasma sintering process. The sintering temperature of the spark plasma is 1250oC. The sintering pressure is 35MPa, the heat preservation time is 35min, the protective gas is argon, the heating rate is 115oC/min；
10) Rolling the multi-layer NiCrAlBNb-based bearing retainer obtained in the step 9), wherein the rolling process is to repeatedly act on a friction film contact layer by using a ceramic-based rolling body to form a nanocrystalline friction film, the applied pressure is 10MPa, the linear velocity is 3m/s, and the temperature is 100 DEGoC, acting for 50min to finally obtain the multilayer nanocrystalline NiCrAlBNb-based bearing retainer material;
FIG. 5 shows the electron microscope morphology of the self-lubricating composite material friction film transition layer and the friction film support layer of the multi-layer nanocrystalline NiCrAlBNb-based bearing retainer in the combined state, which is prepared under the conditions of example 2. FIG. 6 is an electron probe morphology of a friction wear surface of a multi-layer nanocrystalline NiCrAlBNb-based bearing cage self-lubricating composite material prepared under the conditions of example 2. FIG. 3 is a schematic representation of the practice of the present inventionThe friction coefficient curves of the self-lubricating composite materials of the multi-layer nanocrystalline NiCrAlBNb-based bearing retainer prepared in examples 1, 2 and 3. FIG. 4 is a histogram of wear rate of a multi-layer nanocrystalline NiCrAlBNb-based self-lubricating composite material for a bearing cage prepared in examples 1, 2 and 3 of the present invention. As shown in FIGS. 3 and 4, the self-lubricating composite material of the multi-layer nano-crystalline NiCrAlBNb-based bearing retainer prepared in example 2 has a small friction coefficient of about 0.26 and a low wear rate of about 3.24X 10-6mm3/Nm。
Example 3
As shown in figure 1, the design and the preparation method of the self-lubricating composite material of the multi-layer nanocrystalline NiCrAlBNb-based bearing retainer mainly comprise the following steps:
1) weighing ammonium molybdate, silicon powder and cadmium powder according to a molar ratio of 4:3:1, grinding and mixing the ammonium molybdate powder, the silicon powder and the cadmium powder to obtain a plate-shaped crystal original ingredient which is uniformly mixed and has an average particle size of 42.5 mu m; then sintering in a vacuum atmosphere furnace, wherein the sintering temperature is 450 ℃, the heat preservation time is 6.1h, the protective gas is argon, and the oxygen amount is 100ml/min in the sintering process to obtain multilayer platy crystal MoSiCrO;
2) calculating and batching the multilayer platy crystal MoSiCrO obtained in the step 1) with ceramic fiber, carbon fiber, glass fiber, nano white corundum, titanium carbide, tantalum carbide, fullerene, graphene and tungsten disulfide, wherein the proportions of the components of each layer of the multi-component composite regulating agent are different. The multi-element composite regulating agent at the transition layer of the friction film mainly comprises 8% of ceramic fiber, 14% of carbon fiber, 4% of glass fiber, 17.6% of nano white corundum, 13% of titanium carbide, 15% of tantalum carbide, 2.8% of fullerene, 2.4% of graphene, 3.2% of tungsten disulfide and 20% of multilayer platy crystal; the multi-element composite regulating agent on the friction film support layer mainly comprises 8% of ceramic fiber, 15% of carbon fiber, 7% of glass fiber, 14% of nano white corundum, 10% of titanium carbide, 17% of tantalum carbide, 1.4% of fullerene, 1.2% of graphene, 2.2% of tungsten disulfide and 24.2% of multilayer platy crystal; the multi-element composite regulating agent on the contact layer of the friction film mainly comprises 6% of ceramic fiber, 7.2% of carbon fiber, 3.4% of glass fiber, 10.5% of nano white corundum, 15.9% of titanium carbide, 20% of tantalum carbide, 3% of fullerene, 4.5% of graphene, 6.4% of tungsten disulfide and 23.1% of plate-shaped crystal;
3) respectively placing the multi-layer multi-element composite regulation and control ingredients prepared in the step 1) into a pneumatic vacuum vibration mixer for mixing, wherein an outer vibration mixing tank is a quartz tank, a polytetrafluoroethylene tank is arranged in the outer vibration mixing tank, argon flow is used as a mixed power source, and the flow of argon power gas is 125m3The vibration force generated to the tank body is 13000N, the vibration frequency is 50Hz, the vibration time is 50min, and the vacuum degree of the tank body is 2.85 multiplied by 10-2Pa, obtaining the uniformly mixed multi-component composite regulating agent of each layer and storing the regulating agent in a classified manner;
4) weighing Ni, Cr, Al, B, Nb, Si, Co and Y powder according to the mass ratio of 80:16:4:6:2:0.32:0.2: 0.5; weighing Pb, Sn, Ag, Bi and Sb powder according to the mass ratio of 38:27:23:18: 7; and respectively filling NiCrAlBNb powder and PbSnAgBiSb powder into a crucible containing alcohol solution by using vacuum mixing and drying equipment, heating in a vacuum environment, and uniformly mixing and vacuum drying by using alcohol boiling and vacuum evaporation to respectively obtain NiCrAlBNb and PbSnAgBiSb uniformly-mixed powder. Vacuum degree of vacuum mixing and drying is 3.4X 10-2Pa, heating temperature of 42oC, boiling for 36 min;
5) the multi-element composite regulating material obtained in the step 2) is different from NiCrAlBNb-based alloy and PbSnAgBiSb soft alloy in components in each layer structure. The metal matrix is NiCrAlBNb alloy, and the friction film transition layer is composed of NiCrAlBNb alloy, soft alloy PbSnAgBiSb and multi-element composite regulating agent in a mass ratio of 46:18: 30; the friction film supporting layer consists of NiCrAlBNb alloy, soft alloy PbSnAgBiSb and a multi-element composite regulating agent in a mass ratio of 12:11: 76; the friction film contact layer consists of NiCrAlBNb alloy, soft alloy PbSnAgBiSb and a multi-element composite regulating agent in a mass ratio of 4:42: 52;
6) mixing the powder of the NiCrAlBNb base layers and the like in the step 5) by adopting a pneumatic vacuum mixer, wherein the outer tank of the pneumatic vacuum vibration mixer is a quartz tank, and a polytetrafluoroethylene tank is arranged in the quartz tank; the parameters of each layer of pneumatic mixing material are different. The flow rate of argon gas in the transition layer of the friction film is 120m3H, vibration force 5600N, vibration frequency 38Hz, vibration time 135min, and tank vacuum degree of 3.2 × 10-2Pa. The argon gas flow of the friction membrane supporting layer is 123m3The vibration force generated to the tank body is 7800N, the vibration frequency is 52Hz, the vibration time is 110min, and the vacuum degree of the tank body is 3.5 multiplied by 10-2Pa; the flow rate of argon gas in the contact layer of the friction film is 132m3H, generating 5500N vibration force to the tank body, 35Hz vibration frequency, 29min vibration time and 3.4 multiplied by 10 of vacuum degree of the tank body- 2Pa；
7) And (3) respectively loading the uniformly mixed powder of each layer in the step 6) into a hot-pressing forming die to respectively obtain the sheet structures of each layer, such as the metal matrix, the friction film transition layer and the like. The hot-press forming of the friction film transition layer applies pressure of 18MPa, the pressing temperature is 380 ℃, the heat preservation and pressure maintaining time is 240min each time, the air is discharged for 3s every 18min, and the operation is repeatedly carried out for 8 times; hot-press molding the friction membrane supporting layer, wherein the applied pressure is 16MPa, the pressing temperature is 280 ℃, the heat preservation and pressure maintaining time is 140min each time, the air is released for 2s every 40min, and the operation is repeatedly carried out for 5 times; performing hot-press molding on the friction film contact layer, applying pressure of 24MPa, pressing at 175 ℃, keeping the temperature and pressure for 45min each time, deflating for 2s every 15min, and repeating the operation for 4 times;
8) processing the sample of the metal sheet structure obtained in the step 7), turning at a turning speed of 500r/min to obtain a metal sheet with a thickness of each layer and a section diameter of 23 mm; the rotating speed of the grinding process is 135r/min, peripheral burrs and flashes are cleaned by a polishing machine, the rotating speed of electrostatic spraying process equipment is 600r/min, and the subsequent treatment is carried out at the temperature of 75 ℃, so that a sheet with the surface roughness of Ra1.6 and the diameter of 23mm is finally obtained;
9) and (3) sequentially putting the slices with the diameter of 23mm in the step 8) into a graphite mould with the diameter of 25mm, and preparing the NiCrAlBNb-based bearing retainer with the multilayer structure by using a spark plasma sintering process. The sintering temperature of the discharge plasma is 1150oC. Sintering pressure is 32MPa, heat preservation time is 30min, protective gas is argon, heating rate is 110oC/min；
10) Rolling the multi-layer NiCrAlBNb-based bearing retainer obtained in the step 9, wherein the rolling process is to utilize a ceramic-based rolling body to repeatedly act on a friction film contact layer to form a nanocrystalline friction film with the applied pressure of 8MPa, linear velocity of 2.5m/s, temperature of 100oC, acting for 40min to finally obtain the multilayer nanocrystalline NiCrAlBNb-based bearing retainer material;
FIG. 7 is a field emission scanning electron microscope appearance of a friction wear surface of a self-lubricating composite material of a multi-layer nanocrystalline NiCrAlBNb-based bearing retainer prepared in embodiment 3 of the invention. FIG. 8 is a 3D microscopic morphology of the self-lubricating composite material of the multi-layer nano-crystalline NiCrAlBNb-based bearing cage in friction wear, prepared in example 3. FIG. 3 is a friction coefficient curve of a self-lubricating composite material of a multi-layer nanocrystalline NiCrAlBNb-based bearing retainer prepared in examples 1, 2 and 3 of the invention. FIG. 4 is a histogram of wear rate of a multi-layer nanocrystalline NiCrAlBNb-based self-lubricating composite material for a bearing cage prepared in examples 1, 2 and 3 of the present invention; as shown in FIGS. 3 and 4, the self-lubricating composite material of the multi-layer nanocrystalline NiCrAlBNb-based bearing retainer prepared in example 3 has a small friction coefficient of 0.20 and a low wear rate of 3.95X 10-6mm3in/Nm. This shows that the self-lubricating composite material of the multi-layer nanocrystalline NiCrAlBNb-based bearing retainer prepared in example 3 has excellent antifriction and antiwear properties.
The raw materials listed in the invention can realize the invention, and the upper and lower limit values and interval values of the raw materials can realize the invention, and the process parameters of the invention, such as the upper and lower limit values and interval values of frequency, temperature, time, vacuum degree and the like can realize the invention, and the like, but the examples are not listed.

Claims (10)

1. A multilayer nanocrystalline composite structure NiCrAlBNb-based bearing retainer material and a preparation method thereof are characterized in that: the composite material with the multilayer nanocrystalline structure and the NiCrAlBNb as the base body of the bearing retainer is prepared by taking a matrix NiCrAlBNb, soft alloy PbSnAgBiSb and a multi-element composite regulating agent as raw materials and through the process flows of layer-by-layer design, layer-by-layer proportioning, layer-by-layer preparation and superposition molding.
2. The multilayer nanocrystalline composite structure NiCrAlBNb-based bearing cage material according to claim 1, characterized in that: the matrix comprises Ni, Cr, Al, B, Nb, Si, Co and Y elements, and the mass ratio of the elements is (70-80): (5-16): 4-7): 3-6): 2-4): 0.32-0.46: (0.2-0.4): 0.2-0.5); the mass ratio of the elements of the soft alloy PbSnAgBiS is (30-38): (23-27): 23-28): 15-18): 7-10.
3. The multilayer nanocrystalline composite structure NiCrAlBNb-based bearing cage material according to claim 1, characterized in that: the friction film comprises a metal base body, a friction film transition layer, a friction film supporting layer and a friction film contact layer, and the thickness ratio of the metal base body to the friction film transition layer to the friction film contact layer is (45-65): (15-23): (10-20): (5-12).
4. The method for preparing the multi-layer nano-crystal composite structure NiCrAlBNb-based bearing retainer material according to claim 3, is characterized in that: the metal matrix, the friction film transition layer, the friction film supporting layer and the friction film contact layer have different components, and the metal matrix is NiCrAlBNb-based high-temperature alloy; the friction film transition layer comprises NiCrAlBNb alloy, soft alloy PbSnAgBiSb and a multi-element composite regulating agent in a mass ratio of (40-55) to (15-20) to (25-45); the friction film supporting layer comprises a NiCrAlBNb matrix, soft alloy PbSnAgBiSb and a multi-element composite regulating agent, and the mass ratio of the soft alloy PbSnAgBiSb to the multi-element composite regulating agent is (10-15) to (10-13) to (72-80); the friction film contact layer comprises NiCrAlBNb alloy, soft alloy PbSnAgBiSb and a multi-element composite regulating agent in a mass ratio of (3-5) to (40-45) to (50-57).
5. The multilayer nanocrystalline composite structure NiCrAlBNb-based bearing retainer material and the preparation method thereof according to claim 1, is characterized in that: the multi-element composite regulating agent has different proportions in each layer of components, and the friction film transition layer comprises 5-10% of ceramic fiber, 11-15% of carbon fiber, 2.5-5.5% of glass fiber, 16-25% of nano white corundum, 11-15% of titanium carbide, 13-16% of tantalum carbide, 2-3.1% of fullerene, 2-2.5% of graphene, 3-5% of tungsten disulfide and 16-25% of multilayer platy crystal; the friction film supporting layer comprises 6-12% of ceramic fiber, 10-17% of carbon fiber, 4.5-8% of glass fiber, 11-15% of nano white corundum, 8.5-12% of titanium carbide, 14.5-17% of tantalum carbide, 1-1.6% of fullerene, 1-1.3% of graphene, 1.7-2.5% of tungsten disulfide and 22-33% of multilayer platy crystal; the friction film contact layer comprises 2.5-9% of ceramic fiber, 5-8.2% of carbon fiber, 2.5-5% of glass fiber, 10.5-17% of nano white corundum, 12-20% of titanium carbide, 17-24% of tantalum carbide, 3-3.6% of fullerene, 3.6-6% of graphene, 4.5-7.5% of tungsten disulfide and 21.1-26% of multilayer platy crystal.
6. The multilayer nanocrystalline composite structure NiCrAlBNb-based bearing retainer material and the preparation method thereof according to claim 1, is characterized in that: a preparation process of a multilayer platy crystal material MoSiCrO; respectively weighing ammonium molybdate, silicon powder and cadmium powder according to the mol ratio of (3-4) to (2-3) to (1-2), grinding and mixing the ammonium molybdate and other powder to obtain a plate crystal original ingredient which is uniformly mixed and has the average grain diameter of 40-45 mu m; and then sintering in a vacuum atmosphere furnace at the sintering temperature of 400-470 ℃, the heat preservation time of 5.5-6.5h and the protective gas of argon, wherein the oxygen amount is introduced in the sintering process of 75-125ml/min, and the multilayer platy crystal MoSiCrO is obtained.
7. The multilayer nanocrystalline composite structure NiCrAlBNb-based bearing retainer material and the preparation method thereof according to claim 1, is characterized in that: the multi-layer composite structure NiCrAlBNb-based bearing retainer material is obtained through the processes of multi-element plate crystal preparation, material design calculation of each layer, vibration mixing, hot press molding, sample processing, multilayer structure stacking firing, rolling and the like.
8. The multilayer nanocrystalline composite structure NiCrAlBNb-based bearing retainer material and the preparation method thereof according to claim 1, is characterized in that: and (3) performing hot press molding on each layer of material, namely respectively filling the uniformly mixed powder of each layer into a hot press molding die according to the component ratio of the metal matrix, the friction film transition layer, the friction film supporting layer and the friction film contact layer to obtain sheet materials of the metal matrix, the friction film transition layer, the friction film supporting layer and the friction film contact layer, and processing a sample to obtain the composite metal sheet with the diameter of 18-28 mm.
9. The multi-layered nano-crystalline composite NiCrAlBNb-based bearing retainer material and the preparation method thereof according to claim 1, wherein the multi-layered composite structure process flow is characterized in that the metal substrate, the friction film transition layer, the friction film support layer and the friction film contact layer sheet material prepared in the claim 8 are sequentially arranged in a graphite mold with the diameter of 20-30mm, and a spark plasma sintering process is arranged to prepare the multi-layered structure NiCrAlBNb-based bearing retainer material.
10. The multilayer nanocrystalline composite structure NiCrAlBNb-based bearing retainer material and the preparation method thereof according to claim 7, is characterized in that: the rolling treatment process comprises repeatedly acting ceramic-based rolling body on the contact layer of the friction film to form a friction film with nanocrystalline structure, with applied pressure of 5-10MPa, linear velocity of 2-3m/s, and temperature of 100 deg.CoC, the action time is 30-50 min.
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