CN110605879A - Tribological design and preparation method of multilayer composite structure material of NiMoBNb-based separator - Google Patents
Tribological design and preparation method of multilayer composite structure material of NiMoBNb-based separator Download PDFInfo
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- 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
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/10—Metallic powder containing lubricating or binding agents; Metallic powder containing organic material
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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
- B22F3/10—Sintering only
- B22F3/105—Sintering only by using electric current other than for infrared radiant energy, laser radiation or plasma ; by ultrasonic bonding
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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
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B15/00—Layered products comprising a layer of metal
- B32B15/01—Layered products comprising a layer of metal all layers being exclusively metallic
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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
- B22F3/10—Sintering only
- B22F3/105—Sintering only by using electric current other than for infrared radiant energy, laser radiation or plasma ; by ultrasonic bonding
- B22F2003/1051—Sintering only by using electric current other than for infrared radiant energy, laser radiation or plasma ; by ultrasonic bonding by electric discharge
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F2999/00—Aspects linked to processes or compositions used in powder metallurgy
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- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
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- B32B2262/00—Composition or structural features of fibres which form a fibrous or filamentary layer or are present as additives
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Abstract
The invention discloses a multilayer composite structure material of a NiMoBNb-based separator and a preparation method thereof, which takes NiMoBNb matrix powder, a reinforcing material and a multi-element composite material as raw materials, and prepares the multilayer composite structure material of the NiMoBNb-based separator with different thicknesses and material components of each layer through the process flows of vibration and mixing, multilayer structure preforming, surface treatment and layer-by-layer superposition sintering; the separator self-lubricating material can meet the performance requirements of all parts of the separator self-lubricating material, can be used in extremely severe environments with high temperature, strong pressure and high corrosivity, realizes high-performance and reliable work, and has the advantages of bearing capacity, pressure resistance, high temperature resistance and corrosion resistance, and particularly, the tribological performance can effectively meet the required work requirements; the separator has great potential value and wide application prospect in the environment of inconvenient maintenance, repair and lubrication.
Description
Technical Field
The invention relates to the technical field of frictional wear and lubrication of mechanical parts of a centrifugal separator in processing, in particular to a multilayer composite structure material of a NiMoBNb-based separator and a preparation method thereof.
Background
With the rapid development of modern industry, mechanical part separators face a series of extreme service working conditions of ultrahigh temperature, dusty wear, strong corrosion, strong radiation and oil-free and grease-free lubrication in the prior manufacturing field; the main function of the separator is to connect and separate two or more parts, at present, the separator research workers mainly concentrate on the research on the structure of mechanical parts, often neglect the material matching and preparation method of the contact surface of the separator, which causes the separator to face the problems of blockage, corrosion and ultra-high temperature friction damage in the working process; resulting in reduced reliability and service life. The excellent self-lubricating material of the separator should have higher friction coefficient and low abrasion so as to improve the separation efficiency and service life [ Chenyanfei, Zhang Baoyu, Wurenna, Zhengyang Sheng ]. Improvement of waste electrical and electronic equipment based on the overall performance of a friction type electrostatic separator of granular plastics [ J ]; greenwich technology, 2019(04): 171-; the multilayer composite structure material NiMoBNb-based separator self-lubricating material prepared by the invention not only can meet the performance requirements of strong hardness, high heat conductivity and the like of a required mechanical structure, but also has good frictional wear performance, and meanwhile, the separator has the advantages of short preparation period, simple preparation process, easy operation and easy control; the method has potential application value and great development potential in the fields of automobiles, ships, aerospace, energy machinery and advanced manufacturing.
Disclosure of Invention
Aiming at the defects of the prior art, the invention provides a NiMoBNb-based separator multilayer composite structure material and a preparation method thereof, wherein the multilayer composite structure NiMoBNb-based separator self-lubricating material has good mechanical property and excellent antifriction and antiwear properties under the condition of meeting the environmental protection requirement, and is an effective method for solving the problems of easy blockage, corrosion and ultra-high temperature friction damage of a separator product.
The invention adopts the technical scheme that the NiMoBNb-based separator multilayer composite structure material takes NiMoBNb matrix powder, a reinforcing material and a multi-component composite material as raw materials, and is prepared into a NiMoBNb-based separator three-layer composite structure with different thicknesses of layers and different material components through the process flows of material calculation and proportioning, vibration mixing, multilayer structure preforming, sample surface treatment, layer-by-layer superposition sintering and the like, wherein the thickness percentages of a top layer, a middle layer and a bottom layer are respectively 4-9%, 28-42% and 49-65%.
The tribological design and preparation method of the multilayer composite structure material of the NiMoBNb-based separator mainly comprises the following steps:
the NiMoBNb-based separator made of the multilayer composite structure material has different composition mass percentages of the materials of all layers; the top layer comprises 7-10% of NiMoBNb alloy, 25-42% of antiwear agent, 9-13% of heat conduction agent, 15-30% of reinforcing agent and 18-25% of curing agent; the middle layer is composed of 20-30% of NiMoBNb alloy, 10-17% of antiwear agent, 9-12% of heat conduction agent, 28-42% of reinforcing agent and 7-18% of curing agent; the bottom layer is made of pure NiMoBNb alloy material.
The NiMoBNb-based alloy of the multi-layer composite structure material of the separator in the step 1) is composed of Ni, Mo, B, Nb, Cr, Yb, Dy and Y, and the mass ratio of each element in each layer structure is different; the mass ratio of Ni, Mo, B, Nb, Cr, Yb, Dy and Y at the top layer is about 61.5:15:10:8:4:0.6:0.5: 0.4. The mass ratio of the elements in the middle layer is about 64:13:11:7:3.5:0.7:0.4: 0.4; the mass ratio of the elements of Ni, Mo, B, Nb, Cr, Yb, Dy and Y in the bottom layer is (55-65): 10-18): 8-12): 5-9): 3-5): 0.5-0.8): 0.3-0.5): (0.3-0.4).
Designing and weighing the components of the antiwear agent, the heat transfer agent, the reinforcing agent and the curing agent in the step 1) according to the percentage; the top antiwear agent mainly comprises 35-50% of fluorine carbon cerium rare earth, 20-40% of phosphorus yttrium rare earth and 15-25% of WC nano-particles; the heat conduction agent comprises 25-45% of graphene, 25-40% of carbon nano tube and 20-35% of fullerene; the reinforcing agent is composed of 35-50% of graphite fiber, 30-45% of activated carbon fiber and 10-25% of aramid fiber; the curing agent consists of 40-60% of aluminum-based alloy, 15-30% of epoxy cyclohexyl formic acid and 20-30% of bis adipate; wherein the aluminum-based alloy is (33-60) Al (25-35) Pt (17-28) Pb. The middle layer antiwear agent is composed of 37% of fluorine carbon cerium rare earth, 35% of phosphorus yttrium rare earth and 28% of WC nano-particles; the heat conduction agent mainly comprises 46% of graphene, 34% of carbon nano tubes and 20% of fullerene; the reinforcing agent mainly comprises 41% of graphite fiber, 36% of activated carbon fiber and 23% of aramid fiber; the curing agent is composed of 39% aluminum-based alloy, 32% epoxy cyclohexyl formic acid and 29% bis adipate. Wherein the aluminum-based alloy is 52Al32Pt16 Pb.
Respectively mechanically and uniformly mixing the material powder of each layer obtained in the step by adopting a vibration mixer; the vibration frequency is 45-57Hz, the vibration force is 9120-10800N, and the oscillation time is 120-150 min.
Uniformly mixing the ingredients of each layer obtained in the step 4), and performing structure preforming; sequentially loading the uniformly mixed raw materials of each layer into corresponding dies, and compacting by adopting a dry hot press molding process; performing dry hot-press molding at the applied pressure of 8-12MPa, the pressing temperature of 130-; carrying out surface treatment on the pre-formed sample by turning; the turning speed is 780-550 r/min, the turning thickness is 0.8-1.3% of the thickness of each layer, and the grinding speed is 320-453 r/min; cleaning peripheral burrs and flashes by using a polishing machine, and performing surface treatment by using an electrostatic spraying process, wherein the equipment rotation speed is 730-.
Curing heat treatment is carried out on the NiMoBNb-based separator multi-layer composite structure material ingredient obtained in the step 5); firstly heating to 110-.
Sintering ingredients of the multilayer composite structure material of the NiMoBNb-based separator obtained in the step 6), sequentially loading the materials into a die according to a bottom layer, a middle layer and a top layer, and performing multilayer structure combined molding sintering by using discharge plasma; the sintering temperature is 921-1150 ℃, the sintering pressure is 24-27MPa, the heat preservation time is 20-30min, the protective gas is argon, the heating rate is 95-108 ℃/min, and finally the multilayer composite structure NiMoBNb-based separator self-lubricating material is obtained.
The material mixing mode in the step 4) is vibration material mixing, and specifically comprises the steps of firstly utilizing a vibration material mixer to carry out preliminary uniform mixing on reinforcing agents such as graphite fibers, activated carbon fibers and aramid fibers so as to ensure that the composite fibers are uniformly dispersed, then respectively adding other ingredients, and carrying out vibration mixing to obtain uniformly mixed ingredients.
The multilayer composite structure NiMoBNb-based separator self-lubricating material provided by the invention has excellent tribological properties, the friction coefficient is 0.30-0.56, and the wear rate is 2.52-3.63 multiplied by 10-6cm3·N-1·m-1。
Compared with the prior art, the invention has the beneficial effects that:
1. a multilayer composite structure material of a NiMoBNb-based separator is prepared by taking NiMoBNb matrix powder, a graphene reinforcing material and a multi-component composite material as raw materials, and compounding to form the multilayer composite structure material with different thicknesses and reinforcing properties from a bottom layer to a top layer, so that the multilayer composite structure material has excellent mechanical properties and good tribological properties.
2. The NiMoBNb-based alloy content in each layer of the self-lubricating material of the multilayer composite structure NiMoBNb-based separator prepared by the invention is different, each layer has good compatibility, excellent binding performance, compact structure and compact organizational structure, and the method is an effective method for solving the problem of high-temperature peeling and separation between layers of a multilayer structure material.
3. Compared with the traditional separator material, the multilayer composite structure material of the NiMoBNb-based separator is in gradient distribution, so that the relative consumption of raw materials is saved, and the excellent thermodynamic property and friction-reducing and wear-resisting properties of the material are ensured.
4. Considering that the multi-component composite crystal and the graphene reinforced material have good laminated structure and excellent bonding performance, and the like, simultaneously, because the thicknesses of all layers are different and the contents of the reinforced materials are different, the upper layer structure shows stable friction performance and corrosion resistance, the middle layer has larger bearing capacity, and the bottom layer is a substrate layer and has good supporting effect and high-temperature thermal stability.
5. The multilayer composite structure NiMoBNb-based separator self-lubricating material prepared by the invention uses graphite fiber, aramid fiber and glass fiber which have biodegradable performance, so that the health problem can not be caused even if the material is absorbed by a human body, and a large amount of heavy metal raw materials are not used, so that the environment can not be polluted.
Drawings
FIG. 1 is a flow chart of a manufacturing process embodying the present invention.
FIG. 2 is a graph showing the friction coefficient of a multilayer composite structure material of a NiMoBNb-based separator, which is manufactured in examples 1, 2 and 3 of the present invention.
FIG. 3 is a bar graph showing the wear rate of a multilayer composite of a NiMoBNb-based separator made in accordance with examples 1, 2 and 3 of the present invention.
FIG. 4 is an electron microscope topography of the bonding state of the top layer and the middle layer of a NiMoBNb-based separator multilayer composite structure material prepared under the conditions of example 2.
FIG. 5 is an electron probe image of the tribological wear surface of a NiMoBNb-based separator multilayer composite material prepared under the conditions of example 2.
FIG. 6 is a SEM image of the tribological wear surface of a multilayer NiMoBNb-based separator composite material prepared in example 3 of the present invention.
FIG. 7 is a black and white plot of the tribological wear 3D micro-topography of a NiMoBNb-based separator multilayer composite material prepared in example 3.
FIG. 8 is a 3D microscopic morphology grayscale plot of the tribological wear of a multilayer composite material of the NiMoBNb-based separator made in example 3.
Detailed Description
In order to better develop and verify the present invention, the following examples are provided to illustrate 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 10-15N, the speed is 0.15-0.20m/s, the time is 70min and the friction radius is 4.5-5.5 mm.
Example 1
As shown in FIG. 1, the tribology design and the preparation process of the multilayer composite structure material of the NiMoBNb-based separator mainly comprise the following steps:
1) a multilayer structure of the NiMoBNb-based separator is a three-layer composite structure, and the thickness ratio of each layer is that the thickness of a top layer is 4%, the thickness of a middle layer is 35%, and the thickness of a bottom layer is 61% by mass percentage.
2) Calculating the proportion of the required materials according to different mass percentages of each component of the raw materials of the separator; the top layer is 7% of NiMoBNb alloy, 29% of antiwear agent, 9% of heat conduction agent, 30% of reinforcing agent and 25% of curing agent; the middle layer is 20% of NiMoBNb alloy, 10% of antiwear agent, 12% of heat conduction agent, 40% of reinforcing agent and 18% of curing agent. The bottom layer is made of NiMoBNb alloy.
3) Taking materials from each layer of the NiMoBNb alloy according to the mass ratio of the NiMoBNb alloy in each layer of the structure, wherein the NiMoBNb alloy consists of Ni, Mo, B, Nb, Cr, Yb, Dy and Y; the mass ratio of the elements in the top layer is 61.5:15:10:8:4:0.6:0.5:0.4, the mass ratio in the middle layer is 64:13:11:7:3.5:0.7:0.4:0.4, and the mass ratio in the bottom layer is 55:10:8:5:3:0.5:0.3: 0.3.
4) Taking the antiwear agent, the heat conduction agent, the reinforcing agent and the curing agent required by each layer structure according to the step 2) in percentage; the top antiwear agent comprises 35% of fluorine carbon cerium rare earth, 40% of phosphorus yttrium rare earth and 25% of WC nano-particles; the heat conduction agent mainly contains 35% of graphene, 35% of carbon nano tube and 20% of fullerene; the reinforcing agent mainly comprises 35% of graphite fiber, 45% of activated carbon fiber and 20% of aramid fiber; the main components of the curing agent are 40 percent of aluminum-based alloy, 30 percent of epoxy cyclohexyl formic acid and 30 percent of bis adipate; the aluminum-based alloy is 58Al25Pt17 Pb; the middle-layer antiwear agent mainly comprises 37% of fluorine carbon cerium rare earth, 35% of phosphorus yttrium rare earth and 28% of WC nano-particles; the heat conduction agent contains 46% of graphene, 34% of carbon nano tube and 20% of fullerene; the reinforcing agent mainly relates to 41 percent of graphite fiber, 36 percent of activated carbon fiber and 23 percent of aramid fiber; the curing agent comprises 39% aluminum-based alloy, 32% epoxy cyclohexyl formic acid and 29% bis adipate; wherein the aluminum-based alloy is 52Al32Pt16 Pb.
5) Respectively mechanically and uniformly mixing the material powder of each layer obtained in the step by adopting a vibration mixer; the vibration frequency was 45Hz, the vibration force was 9120N, and the oscillation time was 120 min.
6) Sequentially loading the uniformly mixed ingredients of each layer obtained in the step 5) into a die, and performing compaction treatment by using dry hot press molding; performing dry hot press molding at a pressing temperature of 130 ℃ under an applied pressure of 8MPa for 123min, and repeatedly performing 6 times of operations after deflating for 4s every 18 s; the turning speed is 780r/min, the turning thickness is 0.8 percent of the thickness of each layer, and the grinding speed is 320 r/min; and cleaning peripheral burrs and flashes by using a polishing machine, and performing surface treatment by using an electrostatic spraying process at the equipment rotation speed of 730r/min and the temperature of 55 ℃ to obtain the multilayer composite structure material thermosetting ingredient of the NiMoBNb-based separator.
7) And (3) carrying out curing heat treatment on each layer structure processing sample wafer of the multilayer composite structure material obtained in the step 6), namely heating to 110 ℃ in a vacuum drying oven, preserving heat for 2.5h, then heating to 155 ℃ and preserving heat for 4.5h, finally heating to 210 ℃ and preserving heat for 3.5h, and then cooling to room temperature to obtain the sintering ingredient of the multilayer composite structure material of the NiMoBNb-based separator.
8) And (3) sequentially filling the layers of preformed structural materials obtained in the step 7) into a mould according to the sequence of the bottom layer, the middle layer and the top layer, and performing multi-layer structure combined forming sintering by using discharge plasma. The sintering temperature is 921 ℃, the sintering pressure is 24MPa, the heat preservation time is 20min, the protective gas is argon, the heating rate is 95 ℃/min, and finally the multilayer composite structure NiMoBNb-based separator self-lubricating material is obtained.
The hardness of the NiMoBNb-based separator multilayer composite structure material prepared in example 1 is measured according to GB/T4340.1-2009 by adopting an HVS-1000 type digital display Vickers hardness tester, and the hardness is 5.52GPa, and the relative density is 97.8%; FIG. 2 is a graph showing the friction coefficient curve of a multilayer composite structure material of a NiMoBNb-based separator, which is manufactured in examples 1, 2 and 3 of the present invention; FIG. 3 is a bar graph of the wear rate of a multilayer composite of a NiMoBNb-based separator made in accordance with examples 1, 2 and 3 of the present invention; as shown in FIGS. 2 and 3, the multi-layer composite structure material of the NiMoBNb-based separator prepared in example 1 had a relatively low friction coefficient of about 0.56 and a relatively low wear rate of about 2.52X 10-6mm3(iv)/Nm; this shows that a multilayer composite structure material of the NiMoBNb-based separator prepared in example 1 has excellent friction-reducing and wear-resisting properties.
Example 2
As shown in FIG. 1, the tribology design and the preparation process of the multilayer composite structure material of the NiMoBNb-based separator mainly comprise the following steps:
1) a multilayer structure of a NiMoBNb-based separator is a three-layer composite structure, and the thickness percentage of each layer is 7% of the thickness of a top layer, 30% of the thickness of a middle layer and 63% of the thickness of a bottom layer.
2) Calculating the proportion of the required materials according to different mass percentages of each component of the raw materials of the separator; the top layer comprises 8% of NiMoBNb alloy, 32% of antiwear agent, 12% of heat conduction agent, 26% of reinforcing agent and 22% of curing agent; the middle layer comprises 25% of NiMoBNb alloy, 16% of antiwear agent, 9% of heat conduction agent, 36% of reinforcing agent and 14% of curing agent. The bottom layer is pure NiMoBNb alloy.
3) Taking materials from each layer of the NiMoBNb alloy according to the mass ratio of the NiMoBNb alloy in each layer of the structure, wherein the NiMoBNb alloy consists of Ni, Mo, B, Nb, Cr, Yb, Dy and Y. The mass ratio of elements in the top layer is 61.5:15:10:8:4:0.6:0.5:0.4, the mass ratio of elements in the middle layer is 64:13:11:7:3.5:0.7:0.4:0.4, and the mass ratio of elements in the bottom layer is 60:16:11:6.8:5:0.5:0.4: 0.3.
4) Taking the antiwear agent, the heat conduction agent, the reinforcing agent and the curing agent required by each layer structure according to the step 2) in percentage; the antiwear agent on the top layer comprises 42 percent of fluorine carbon cerium rare earth, 38 percent of phosphorus yttrium rare earth and 20 percent of WC nano-particles; the heat conduction agent comprises 25% of graphene, 40% of carbon nano tubes and 35% of fullerene; the reinforcing agent mainly comprises 43% of graphite fiber, 32% of activated carbon fiber and 25% of aramid fiber; the curing agent comprises 50% of aluminum-based alloy, 24% of epoxy cyclohexyl formic acid and 26% of bis adipate; the aluminum-based alloy is 50Al30Pt20 Pb; the middle layer antiwear agent comprises 37% of fluorine carbon cerium rare earth, 35% of phosphorus yttrium rare earth and 28% of WC nano-particles; the heat conduction agent mainly comprises 46% of graphene, 34% of carbon nano tube and 20% of fullerene; the reinforcing agent comprises 41% of graphite fiber, 36% of activated carbon fiber and 23% of aramid fiber. The curing agent mainly comprises 39% of aluminum-based alloy, 32% of epoxy cyclohexyl formic acid and 29% of bis adipate; the aluminum-based alloy is 52Al32Pt16 Pb.
5) Respectively mechanically and uniformly mixing the material powder of each layer obtained in the step by adopting a vibration mixer; the vibration frequency was 52Hz, the vibration force was 10000N, and the oscillation time was 140 min.
6) Sequentially loading the uniformly mixed ingredients of each layer obtained in the step 5) into a die, and performing compaction treatment by using dry hot press molding; performing dry hot press molding under the pressure of 10MPa at the pressing temperature of 145 ℃, keeping the temperature and pressure for 138min, and repeatedly performing 7 times of operations with 5s of air release every 22 s; the turning speed is 856r/min, the turning thickness is 1.1 percent of the thickness of each layer, and the grinding speed is 415 r/min; and cleaning peripheral burrs and flashes by using a polishing machine, and performing surface treatment by using an electrostatic spraying process at the equipment rotating speed of 825r/min and the temperature of 60 ℃ to obtain a processing sample wafer of each layer structure.
7) Curing heat treatment is carried out on the processing sample wafer of each layer structure of the multilayer composite structure material obtained in the step 6), namely the temperature is raised to 120 ℃ in a vacuum drying oven and is preserved for 3.2h, then the temperature is raised to 175 ℃ and is preserved for 5.5h, finally the temperature is raised to 220 ℃ and is preserved for 4.2h, and then the temperature is cooled to room temperature, so as to obtain the NiMoBNb-based separator self-lubricating material of the multilayer composite structure material; FIG. 4 is an electron microscope topography of the bonding state of the top layer and the middle layer of a NiMoBNb-based separator multilayer composite structure material prepared under the conditions of example 2.
8) Sequentially filling the layers of preformed structural materials obtained in the step 7) into a die according to the bottom layer, the middle layer and the top layer, and performing multi-layer structure combined forming sintering by using discharge plasma; the sintering temperature is 1000 ℃, the sintering pressure is 25MPa, the heat preservation time is 25min, the protective gas is argon, the heating rate is 100 ℃/min, and finally the multilayer composite structure NiMoBNb-based separator self-lubricating material is obtained.
The hardness of the NiMoBNb-based separator multilayer composite structure material prepared in example 2 is measured by adopting an HVS-1000 type digital Vickers hardness tester according to GB/T4340.1-2009, and the hardness is 5.44GPa, and the relative density is 97.5%; FIG. 5 is an electron probe view of the tribological wear surface of a NiMoBNb-based separator multilayer composite material prepared under the conditions of example 2; FIG. 2 is a graph showing the friction coefficient curve of a multilayer composite structure material of a NiMoBNb-based separator, which is manufactured in examples 1, 2 and 3 of the present invention; FIG. 3 is a bar graph of the wear rate of a multilayer composite of a NiMoBNb-based separator made in accordance with examples 1, 2 and 3 of the present invention; as shown in FIGS. 2 and 3, the multi-layer composite structure material of the NiMoBNb-based separator prepared in example 1 had a relatively low friction coefficient of about 0.37 and a relatively low wear rate of 3.37X 10-6mm3in/Nm. This shows that the multilayer composite structure material of the NiMoBNb-based separator prepared in example 2 has excellent friction-reducing and wear-resisting properties.
Example 3
As shown in FIG. 1, the tribology design and the preparation process of the multilayer composite structure material of the NiMoBNb-based separator mainly comprise the following steps:
1) a multilayer structure of the NiMoBNb-based separator is a three-layer composite structure, and the thickness ratio of each layer is that the thickness of a top layer is 9%, the thickness of a middle layer is 42%, and the thickness of a bottom layer is 49% by mass percentage.
2) Calculating the ratio of the required raw materials according to different mass percentages of each layer of components of the raw materials of the separator; the top layer comprises 10% of NiMoBNb alloy, 42% of antiwear agent, 9% of heat conduction agent, 21% of reinforcing agent and 18% of curing agent; the middle layer comprises 20% of NiMoBNb alloy, 17% of antiwear agent, 10% of heat conduction agent, 42% of reinforcing agent and 11% of curing agent. The bottom layer is made of NiMoBNb alloy.
3) Taking materials from each layer of the NiMoBNb alloy according to the mass ratio of the NiMoBNb alloy in each layer of the structure, wherein the NiMoBNb alloy consists of Ni, Mo, B, Nb, Cr, Yb, Dy and Y; the mass ratio of the elements in the top layer is 61.5:15:10:8:4:0.6:0.5:0.4, the mass ratio of the elements in the middle layer is 64:13:11:7:3.5:0.7:0.4:0.4, and the mass ratio of the elements in the bottom layer is 65:18:12:9:5:0.8:0.5: 0.4.
4) Taking the antiwear agent, the heat conduction agent, the reinforcing agent and the curing agent required by each layer structure according to the step 2) in percentage; the top layer antiwear agent mainly comprises 50% of fluorine carbon cerium rare earth, 35% of phosphorus yttrium rare earth and 15% of WC nano-particles; the heat conduction agent mainly comprises 45% of graphene, 25% of carbon nano tubes and 30% of fullerene; the reinforcing agent mainly comprises 50% of graphite fiber, 40% of activated carbon fiber and 10% of aramid fiber; the curing agent mainly comprises 60 percent of aluminum-based alloy, 15 percent of epoxy cyclohexyl formic acid and 25 percent of bis adipate; wherein the aluminum-based alloy material is 60Al20Pt20 Pb. The middle layer antiwear agent comprises 37% of fluorine carbon cerium rare earth, 35% of phosphorus yttrium rare earth and 28% of WC nano-particles; the heat conduction agent comprises 46% of graphene, 34% of carbon nano tubes and 20% of fullerene; the reinforcing agent comprises 41% of graphite fiber, 36% of activated carbon fiber and 23% of aramid fiber; the curing agent consists essentially of 39% aluminum-based alloy, 32% epoxy cyclohexyl formic acid and 29% bis adipate. Wherein the aluminum-based alloy is 52Al32Pt16 Pb.
5) Respectively mechanically and uniformly mixing the material powder of each layer obtained in the step by adopting a vibration mixer; the vibration frequency was 57Hz, the vibration force was 10800N, and the oscillation time was 150 min.
6) Sequentially loading the uniformly mixed ingredients of each layer obtained in the step 5) into a die, and performing compaction treatment by using dry hot press molding; performing dry hot press molding at a pressing temperature of 163 ℃ for 149min under 12MPa, and repeatedly performing 8 times of operations after 6s of air release every 25 s; the turning speed is 966r/min, the turning thickness is 1.3 percent of the thickness of each layer, and the grinding speed is 453 r/min; and cleaning peripheral burrs and flashes by using a polishing machine, and performing surface treatment by using an electrostatic spraying process at the equipment rotating speed of 890r/min and the temperature of 65 ℃ to obtain the processing pre-molded sample wafer of each layer structure.
7) Curing heat treatment is carried out on the processing sample wafer of each layer structure of the multilayer composite structure material obtained in the step 6), namely, the temperature is firstly raised to 130 ℃ in a vacuum drying oven and is preserved for 3.5h, then the temperature is raised to 185 ℃ and is preserved for 6.5h, finally the temperature is raised to 230 ℃ and is preserved for 4.5h, and then the temperature is cooled to room temperature, so as to obtain the NiMoBNb-based separator self-lubricating material of the multilayer composite structure material; FIG. 4 is an electron microscope topography of the bonding state of the top layer and the middle layer of a NiMoBNb-based separator multilayer composite structure material prepared under the conditions of example 2.
8) Sequentially filling the layers of preformed structural materials obtained in the step 7) into a die according to the bottom layer, the middle layer and the top layer, and performing multi-layer structure combined forming sintering by using discharge plasma; the sintering temperature is 1150 ℃, the sintering pressure is 27MPa, the heat preservation time is 30min, the protective gas is argon, the heating rate is 108 ℃/min, and finally the multilayer composite structure NiMoBNb-based separator self-lubricating material is obtained.
The hardness of the NiMoBNb-based separator multilayer composite structure material prepared in example 3 is measured according to GB/T4340.1-2009 by adopting an HVS-1000 type digital display Vickers hardness tester, wherein the hardness is 5.54GPa, and the relative density is 97.2%; FIG. 6 is a SEM image of the tribological wear surface of a multilayer NiMoBNb-based separator composite material prepared in example 3 of the present invention; FIG. 7 is a 3D topographical view of the tribological wear of the multi-layer composite material of the NiMoBNb-based separator prepared in example 3; FIG. 2 is a graph showing the friction coefficient curve of a multilayer composite structure material of a NiMoBNb-based separator, which is manufactured in examples 1, 2 and 3 of the present invention; FIG. 3 is a bar graph of the wear rate of a multilayer composite of a NiMoBNb-based separator made in accordance with examples 1, 2 and 3 of the present invention; as shown in FIGS. 2 and 3, the multi-layer composite structure material of the NiMoBNb-based separator prepared in example 3 had a relatively low friction coefficient of about 0.30 and a relatively low wear rate of about 3.63X 10-6mm3(iv)/Nm; this shows that the multilayer composite structure material of the NiMoBNb-based separator prepared in example 3 has excellent friction-reducing and wear-resisting properties.
The above description is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, many modifications and changes can be made without departing from the inventive concept of the present invention, and these modifications and changes are within the scope of the present invention.
Claims (10)
1. A friction design and a preparation method of a multilayer composite structure material of a NiMoBNb-based separator are characterized in that: the NiMoBNb-based separator self-lubricating material is a multi-layer composite structure material NiMoBNb-based separator self-lubricating material which is formed by compounding NiMoBNb matrix powder, performance-enhancing material graphene and a multi-component composite material serving as raw materials, wherein the thicknesses of the layers from the bottom layer to the top layer are different, and the components are different and the contents are different.
2. The tribological design and preparation method of a multilayer composite structure material of a NiMoBNb-based separator according to claim 1, characterized in that: and (3) sequentially carrying out weighing, material proportioning, vibration mixing, multilayer structure preforming, sample surface treatment and layer stacking and sintering on each layer of raw materials to obtain the NiMoBNb-based separator self-lubricating material with the multilayer composite structure.
3. The tribological design and preparation method of a multilayer composite structure material of a NiMoBNb-based separator according to claim 1, characterized in that: the composite material is formed by compounding three layers, wherein the thickness percentages of a top layer, a middle layer and a bottom layer are 4-9%, 28-42% and 49-65%.
4. The tribological design and the preparation method of the multilayer composite structure material of the NiMoBNb-based separator according to claim 3, wherein each layer of the structural components consists of NiMoBNb alloy, antiwear agent, heat conduction agent, reinforcing agent and curing agent.
5. The tribology design and the manufacturing method of the multilayer composite structure material of the NiMoBNb-based separator according to claim 4, wherein the raw material weight percentages of each layer of the separator are different; the top layer comprises 7-10% of NiMoBNb alloy, 25-42% of antiwear agent, 9-13% of heat conduction agent, 15-30% of reinforcing agent and 18-25% of curing agent; the middle layer is composed of 20-30% of NiMoBNb alloy, 10-17% of antiwear agent, 9-12% of heat conduction agent, 28-42% of reinforcing agent and 7-18% of curing agent; the bottom layer component is pure NiMoBNb alloy material.
6. The tribological design and manufacturing method of the multilayer composite structure material of the NiMoBNb-based separator according to claim 5, wherein the NiMoBNb alloy is composed of Ni, Mo, B, Nb, Cr, Yb, Dy and Y, and the mass ratios of the elements in each layer are different; the mass ratio of the elements on the top layer is about 61.5:15:10:8:4:0.6:0.5: 0.4; the mass ratio of the elements in the middle layer is about 64:13:11:7:3.5:0.7:0.4: 0.4; the mass ratio of the elements in the bottom layer is (55-65): (10-18): 8-12): 5-9): 3-5): 0.5-0.8): 0.3-0.5): 0.3-0.4.
7. The tribological design and preparation method of a multilayer composite structure material of NiMoBNb-based separator according to claim 5, characterized in that it is composed of antiwear agent, heat conduction agent, reinforcing agent and curing agent with different components in each layer structure; the top layer is an antiwear agent mainly comprising 35-50% of fluorine carbon cerium rare earth, 20-40% of phosphorus yttrium rare earth and 15-25% of WC nano-particles; the heat conduction agent comprises 25-45% of graphene, 25-40% of carbon nano tube and 20-35% of fullerene; the reinforcing agent is composed of 35-50% of graphite fiber, 30-45% of activated carbon fiber and 10-25% of aramid fiber; the curing agent consists of 40-60% of aluminum-based alloy, 15-30% of epoxy cyclohexyl formic acid and 20-30% of bis adipate; wherein the aluminum-based alloy is (33-60) Al (25-35) Pt (17-28) Pb; the middle layer antiwear agent is composed of 37% of fluorine carbon cerium rare earth, 35% of phosphorus yttrium rare earth and 28% of WC nano-particles; the heat conduction agent mainly comprises 46% of graphene, 34% of carbon nano tubes and 20% of fullerene; the reinforcing agent component comprises 41% of graphite fiber, 36% of activated carbon fiber and 23% of aramid fiber; the curing agent consists of 39 percent of aluminum-based alloy, 32 percent of epoxy cyclohexyl formic acid and 29 percent of bis adipate; wherein the aluminum-based alloy is 52Al32Pt16 Pb.
8. The tribological design and preparation method of the multilayer composite structure material of the NiMoBNb-based separator according to claim 5, wherein the pre-forming process of each layer of structure comprises the steps of sequentially filling the uniformly mixed powder of each layer into a mold, and then hot-pressing and curing heat treatment; performing dry hot-press molding, wherein the applied pressure is 8-12MPa, the pressing temperature is 130-; turning the preformed sample, wherein the turning rotating speed is 780-966r/min, the turning thickness is 0.8-1.3% of the thickness of each layer, and the rotating speed in the grinding process is 320-453 r/min; and cleaning burrs and flashes by using a polishing machine, and treating the surface of the sample by using an electrostatic spraying process at the equipment rotation speed of 730-.
9. The tribological design and preparation method of a multilayer composite structure material of a NiMoBNb-based separator according to claim 8, characterized in that: sequentially loading the sintered samples of each layer into a die according to the sequence of the bottom layer, the middle layer and the top layer, and performing combined molding sintering of the multilayer structure by using discharge plasma; the sintering temperature is 921-1150 ℃, the sintering pressure is 24-27MPa, the heat preservation time is 20-30min, the protective gas is argon, the heating rate is 95-108 ℃/min, and the multilayer composite structure NiMoBNb-based separator self-lubricating material is obtained.
10. The tribological design and preparation method of a multilayer composite structure material of a NiMoBNb-based separator according to claim 8, characterized in that: curing heat treatment process of the curing agent; the method comprises the steps of heating to 110-.
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