CN115106533A - Organic/inorganic gradient composite material for oil-retaining bearing and preparation method thereof - Google Patents
Organic/inorganic gradient composite material for oil-retaining bearing and preparation method thereof Download PDFInfo
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- 238000002360 preparation method Methods 0.000 title claims abstract description 15
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- 229910052802 copper Inorganic materials 0.000 claims abstract description 114
- 239000011148 porous material Substances 0.000 claims abstract description 46
- 239000011159 matrix material Substances 0.000 claims abstract description 32
- 239000000314 lubricant Substances 0.000 claims abstract description 31
- 238000005245 sintering Methods 0.000 claims abstract description 29
- 238000000034 method Methods 0.000 claims abstract description 26
- 239000002994 raw material Substances 0.000 claims abstract description 18
- 239000002253 acid Substances 0.000 claims abstract description 6
- 238000004519 manufacturing process Methods 0.000 claims abstract 2
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- 229910052751 metal Inorganic materials 0.000 claims description 50
- 239000002184 metal Substances 0.000 claims description 50
- 239000000843 powder Substances 0.000 claims description 34
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 30
- 238000001291 vacuum drying Methods 0.000 claims description 30
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- 230000003746 surface roughness Effects 0.000 claims description 9
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- 238000009826 distribution Methods 0.000 abstract description 11
- 238000013461 design Methods 0.000 abstract description 3
- 239000002243 precursor Substances 0.000 abstract description 3
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- 238000012360 testing method Methods 0.000 description 14
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- 229910000838 Al alloy Inorganic materials 0.000 description 12
- 229910052782 aluminium Inorganic materials 0.000 description 12
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 11
- 239000002245 particle Substances 0.000 description 9
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- 238000006243 chemical reaction Methods 0.000 description 8
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- 238000004140 cleaning Methods 0.000 description 7
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- 229910021641 deionized water Inorganic materials 0.000 description 7
- 238000001035 drying Methods 0.000 description 7
- 238000011049 filling Methods 0.000 description 7
- 239000010439 graphite Substances 0.000 description 7
- 229910002804 graphite Inorganic materials 0.000 description 7
- 238000004321 preservation Methods 0.000 description 7
- 238000002474 experimental method Methods 0.000 description 6
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- 230000001050 lubricating effect Effects 0.000 description 5
- 238000012876 topography Methods 0.000 description 5
- 239000002041 carbon nanotube Substances 0.000 description 4
- 229910021393 carbon nanotube Inorganic materials 0.000 description 4
- 238000010586 diagram Methods 0.000 description 4
- 229910017767 Cu—Al Inorganic materials 0.000 description 3
- 229910010293 ceramic material Inorganic materials 0.000 description 3
- 230000007797 corrosion Effects 0.000 description 3
- 238000005260 corrosion Methods 0.000 description 3
- 238000005086 pumping Methods 0.000 description 3
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 2
- 238000002441 X-ray diffraction Methods 0.000 description 2
- KUNSUQLRTQLHQQ-UHFFFAOYSA-N copper tin Chemical compound [Cu].[Sn] KUNSUQLRTQLHQQ-UHFFFAOYSA-N 0.000 description 2
- 238000007654 immersion Methods 0.000 description 2
- 239000002861 polymer material Substances 0.000 description 2
- 238000012545 processing Methods 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 239000012748 slip agent Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 239000000758 substrate Substances 0.000 description 2
- 239000010724 circulating oil Substances 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 230000003247 decreasing effect Effects 0.000 description 1
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- 238000011161 development Methods 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 239000002905 metal composite material Substances 0.000 description 1
- 239000007769 metal material Substances 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 229920003023 plastic Polymers 0.000 description 1
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- 238000007711 solidification Methods 0.000 description 1
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- 238000002490 spark plasma sintering Methods 0.000 description 1
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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
- B22F7/002—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 porous nature
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
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- 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
- B22F3/02—Compacting only
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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
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/24—After-treatment of workpieces or articles
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/24—After-treatment of workpieces or articles
- B22F3/26—Impregnating
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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
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/04—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23F—NON-MECHANICAL REMOVAL OF METALLIC MATERIAL FROM SURFACE; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL; MULTI-STEP PROCESSES FOR SURFACE TREATMENT OF METALLIC MATERIAL INVOLVING AT LEAST ONE PROCESS PROVIDED FOR IN CLASS C23 AND AT LEAST ONE PROCESS COVERED BY SUBCLASS C21D OR C22F OR CLASS C25
- C23F1/00—Etching metallic material by chemical means
- C23F1/10—Etching compositions
- C23F1/14—Aqueous compositions
- C23F1/16—Acidic compositions
- C23F1/20—Acidic compositions for etching aluminium or alloys thereof
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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
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/04—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
- B22F2009/043—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling by ball milling
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Abstract
The invention discloses an organic/inorganic gradient composite material for an oil-retaining bearing and a preparation method thereof. The composite material comprises a gradient porous copper matrix and an organic lubricant poured in pores of the gradient porous copper matrix; wherein: the gradient porous copper matrix is of a multilayer structure, and the porosity or pore diameter of each layer of porous copper is in gradient change. The invention selects a copper-aluminum or copper-iron multilayer alloy system, and prepares the gradient porous copper matrix by gradient design of each layer of precursor raw material components, gradient lamination, sintering and dealloying in acid. The composite material has small aperture, large specific surface area, uniform pore distribution and controllable porosity, the oil content of the composite material can reach 5-35%, the oil retention rate is up to more than 50%, and the composite material has good mechanical property and potential application value in the field of lubrication; meanwhile, the preparation method has the advantages of simple equipment, stable process, high production efficiency and positive engineering application value.
Description
Technical Field
The invention belongs to the technical field of oil-retaining bearings, and particularly relates to an organic/inorganic gradient composite material for an oil-retaining bearing and a preparation method thereof.
Background
The porous material matrix widely applied at present comprises a metal material, a ceramic material and a polymer material. The porous ceramic material has stable chemical properties, good high-temperature resistance and corrosion resistance, but the porous ceramic material has too high density and small impact strength; the porous polymer material has the advantages of low density and plastic deformation, but has poor heat conduction performance and is easy to soften and lose efficacy under high-speed friction.
The porous metal composite material containing the lubricant has the advantages of light weight, low noise, strong corrosion resistance, good lubricating property, capability of circulating oil supply and the like, and is a novel lubricating material capable of meeting special working conditions. For the existing porous retainer material with a single pore structure, the lubricating property and the mechanical property are two mutually restricted aspects, when the oil content is to be improved, the porosity and the pore diameter are generally increased, so that the mechanical strength and the processing manufacturability are reduced, if the mechanical strength and the oil retention rate are increased, the porosity and the pore diameter need to be reduced, the lubricating property is reduced, and the bonding strength of an interface is reduced along with the addition of a lubricant. How to achieve high oil content, high oil retention rate, good mechanical properties and good processing manufacturability of a high-speed bearing retainer material becomes a bottleneck problem restricting the development of a high-speed bearing, needs to be overcome, solves the problems, needs to explore a new porous lubricant-containing composite material meeting the use requirement, and the existing porous metal with a single pore structure cannot meet the requirement of complex functionality, so that the research of the porous metal bearing is developed towards the direction of controlling and realizing a gradient pore structure.
Hao Du et al prepared porous copper with elongated holes by a radial solidification method and studied the oil retention capacity of the porous copper, but the prepared porous copper had poor oil retention; L/Ju/et al prepared a carbon nanotube reinforced porous copper-tin oil-retaining bearing by a powder metallurgy method. The coated carbon nanotubes can improve the mechanical properties and oil content of the porous copper-tin oil-retaining bearing. When the carbon nanotube content was 1 wt%, the oil content reached 23.42% and then decreased. Adding too many carbon nanotubes reduces the pore structure and reduces the mechanical properties and oil content of the porous bearing. X/aole/L/et al used spark plasma sintering to obtain N/T/alloys of different porosities. A porous N/T/alloy having excellent tribological properties and shape memory properties is obtained, but its oil content, oil retention is not high. At present, researches are mainly carried out on the friction coefficient and the wear rate of the porous oil-containing composite material, the porous material with high oil content is pursued, and the oil retention rate is rarely considered.
Therefore, there is an urgent need to find a porous material having high oil content, high oil retention and good mechanical properties at the same time.
Disclosure of Invention
The technical problem to be solved by the invention is as follows: aiming at the defects of low oil content and low oil retention rate of single-pore porous metal prepared by the traditional method, the organic/inorganic gradient composite material for the oil-containing bearing and the preparation method thereof are provided.
In order to solve the technical problem, the invention adopts the following technical scheme:
providing an organic/inorganic gradient composite material for an oil-impregnated bearing, comprising a gradient porous copper matrix and an organic lubricant poured in pores of the gradient porous copper matrix; wherein:
the gradient porous copper matrix is of a multilayer structure, and the porosity or pore diameter of each layer of porous copper is in gradient change.
According to the scheme, in the gradient porous copper matrix, the porosity of each layer of porous copper is in gradient change between 0% and 89.56%, and the pore diameter is in gradient change between 0.1 μm and 10 μm.
The preparation method of the organic/inorganic gradient composite material for the oil-retaining bearing comprises the following steps:
1) taking copper powder and active metal powder as raw materials, respectively weighing the copper powder and the active metal powder according to the designed layer number of each layer, and fully mixing, wherein the element content ratio of the copper powder and the active metal powder in the raw materials of each layer is changed in a gradient manner, and the active metal powder is one of aluminum powder and iron powder;
2) stacking each layer of raw material mixed powder obtained in the step 1), pressing and forming, preparing a copper alloy block by using a powder metallurgy technology, and removing active metal powder to prepare a gradient porous copper matrix;
3) soaking the gradient porous copper matrix obtained in the step 2) in an organic lubricant to enable the organic lubricant to be soaked in pores of the porous copper matrix, and obtaining the organic/inorganic gradient composite material for the oil-retaining bearing.
According to the scheme, in the step 1), the particle size of the copper powder is 0.2-5 microns, and the particle size of the aluminum powder is 0.2-5 microns.
According to the scheme, in the step 1), the mass fraction of copper powder in each layer of raw materials is not less than 10%, and the copper powder is in gradient change.
According to the scheme, in the step 1), the fully mixing mode of the copper powder and the active metal powder is ball milling.
According to the scheme, in the step 2), in the powder metallurgy technology, the specific sintering process is as follows: the heating rate is 50-200 ℃/m//, the sintering temperature is 400-.
According to the scheme, in the step 2), the step of removing the active metal powder comprises the following steps: and (3) putting the copper alloy block into a container filled with an acid solution, and reacting at a constant temperature until no bubbles are generated, thus obtaining the gradient porous copper matrix.
Preferably, the acid solution is a sulfuric acid solution, more preferably, the sulfuric acid solution has a concentration of 5 to 25 wt%.
Preferably, the constant temperature is 60-95 ℃.
According to the scheme, in the step 3), the organic lubricant is one or more of liquid paraffin, polyolefin, mineral oil, polyethylene glycol, polyalkylcyclopentane, diester oil and fully synthetic oil.
According to the scheme, in the step 3), the gradient porous copper matrix is soaked in the organic lubricant and soaked under a vacuum drying condition. Preferably, the vacuum degree under the vacuum condition is more than or equal to 0.08 MPa; the soaking temperature is 40-150 ℃, and the soaking time is 2-24 hours.
According to the scheme, in the step 3), before the gradient porous copper matrix is soaked in the organic lubricant, polishing treatment is carried out until the surface roughness Ra is less than or equal to 1 mu m.
According to the scheme, the gradient porous copper matrix has the following performance indexes: the pore diameter is 0.1-10 mu m, the porosity is 0-89.56%, the compressive strength is 0.89-206.14MPa, the oil content is 5-35%, and the oil retention rate is more than 50%.
Compared with the prior art, the invention has the following main advantages:
1. the invention provides an organic/inorganic gradient composite material for an oil-retaining bearing, which takes multi-layer porous copper as a substrate, wherein each layer of the aperture or porosity of the porous copper substrate is in gradient change, the high-porosity layer stores oil, the low-porosity and small-aperture layer enhances the capillary force to realize high oil retention rate, and the obtained composite material has small aperture, large specific surface area, uniform pore distribution and controllable porosity, the oil retention rate of the composite material can reach 5-35%, the oil retention rate of the composite material is up to more than 50%, and the composite material has good mechanical properties and potential application value in the lubrication field.
2. The invention provides a preparation method of an organic/inorganic gradient composite material for an oil-retaining bearing, which is characterized in that the heat conductivity, the dimensional stability, the chemical stability and the corrosion resistance of porous copper are superior to those of porous iron and porous aluminum, a copper-aluminum or copper-iron multilayer alloy system is selected, a gradient porous copper matrix is prepared by performing gradient design, gradient lamination and sintering on each layer of precursor raw material components and dealloying in acid, and the porosity and the pore structure of the porous copper can be controlled by adjusting the phase composition and the raw material size of each layer in the alloy; the obtained gradient composite material has high oil content and high oil retention rate, and certain strength is ensured.
Drawings
FIG. 1 is a process flow diagram of an embodiment of the invention.
Fig. 2 is an XRD pattern (left diagram) of a sample of copper-aluminum alloy and pure copper with Cu contents of 40%, 50% and 60% respectively in the copper-aluminum alloy block prepared in example 1 of the present invention and a control group, and the right diagram is an enlarged view thereof.
FIG. 3 is XRD patterns of samples after aluminum removal from the Cu-Al alloy samples with Cu contents of 40%, 50% and 60% respectively in the Cu-Al alloy blocks prepared in example 1 of the present invention and the control group.
FIG. 4 is a polished microstructure (BSE) of a cross-section of a Cu-Al alloy block prepared in example 1 of the present invention.
FIG. 5 is a micro-topography of a gradient porous copper matrix prepared in example 1 of the present invention, wherein a is a Cu sample gradient 40 Al 60 A macro topography after layer dealloying, fig. a-1 is a partial enlarged view of fig. a; FIG. b shows Cu 50 Al 50 A macro topography after layer dealloying, fig. b-1 is a partial enlarged view of fig. b; FIG. c is Cu 60 Al 40 A macro topography after layer dealloying, fig. c-1 is a partial enlargement of fig. c; fig. d is a diagram of the macro-topography of the pure copper layer after dealloying, and fig. d-1 is a partial enlargement of fig. d.
FIG. 6 is a graph of porosity after removal of aluminum for comparative examples of 30%, 40%, 50%, 60%, and 70% Cu content in example 1.
FIG. 7 is a graph of the oil content after removing aluminum and the oil retention after centrifugal oil throwing at 1K-4K of the copper-aluminum alloy samples with Cu contents of 40%, 50% and 60% respectively in the gradient porous copper matrix prepared in example 1 of the present invention and the control group.
FIG. 8 is a graph of the coefficient of friction at load 6N rate of 200mm/m// reciprocating and the dry coefficient of friction without oil immersion after preparation of the gradient porous copper matrix impregnated slip agent PAO10 of example 1 of the present invention.
Detailed Description
In the embodiment of the invention, Plasma Activated Sintering (PAS) is adopted, mixed powder with different contents is sintered to obtain a gradient component alloy block body in a laminated mode, the gradient component alloy block body is cleaned and immersed into sulfuric acid solution for dealloying, active components in the alloy are removed by utilizing the chemical reaction of the active components in the sulfuric acid solution, so that gradient porous copper with better strength is obtained, the porous copper is immersed into lubricating oil, and the organic/inorganic gradient composite material of the oil-containing bearing is obtained, wherein the process flow is shown in figure 1. By utilizing the gradient design, the contradiction among the oil content, the oil retention rate and the mechanical strength of the existing porous oil-containing material is solved. The invention can produce products with large size, has simple process and low cost and is easy for industrialization.
The present invention will be further described with reference to the following examples and drawings, but the present invention is not limited thereto.
Example 1
A preparation method of an organic/inorganic gradient composite material for an oil-impregnated bearing is provided, which comprises the following steps:
1) weighing copper powder and aluminum powder with the purity of more than or equal to 99.0% and the particle size of 0.2-5 mu m according to the atomic ratio of 100:0, 60:40, 50:50 and 40:60 respectively, and ball-milling the mixed raw material powder on a light low-energy ball mill at the speed of 240 revolutions per minute for 24 hours to uniformly mix the composite powder;
2) and (2) filling the composite powder into a graphite mold by adopting a layering method, prepressing the sample for 10 minutes under the pressure of 5MPa, and then performing Plasma Activated Sintering (PAS), wherein the vacuum degree is less than or equal to 10Pa, the sintering temperature is 530 ℃, the heating rate is 50 ℃/m//, the heat preservation time is 5 minutes, and the sintering pressure is 50MPa, so that the copper-aluminum alloy block is obtained. As shown in FIG. 2, the phases of the prepared gradient sample are superposed by single-layer phases without impurities and are accurate. In fig. 4, it is shown that the phase distribution of the precursor alloy of the gradient sample is uniform and the interface bonding is good. Wherein the Cu contents obtained by sintering under the same conditions were 30% (Cu) 30 Al 70 )、40％(Cu 40 Al 60 )、50％(Cu 50 Al 50 )、60％(Cu 40 Al 60 ) And 70％(Cu 70 Al 30 ) The copper-aluminum alloy sample and the pure copper are used as control groups.
3) Clean alloy is put into 5 wt% H 2 SO 4 The container was placed in a constant temperature water bath (90 ℃) and the time was recorded. Observing bubbles generated by the reaction of the active metal aluminum in the container and the sulfuric acid solution, finding that no bubbles are generated in the solution after 48 hours, then taking out the metal block, and repeatedly washing the metal block with alcohol and deionized water to obtain the gradient porous copper matrix. As shown in FIG. 5, porous copper with a gradient porosity distribution was obtained, and the pore diameters of the gradient layers were uniformly distributed. As shown in FIG. 3, the obtained porous metal is a pure copper phase, the porosity of the obtained porous metal is 62.25%, the pore size distribution is in the range of 0.2-0.4 μm, and the compressive strength is 56.18 MPa. Wherein, the control group of the step 2) is used as the control group to carry out XRD test after being subjected to dealloying under the same conditions as the step 3). FIG. 7 shows that the Cu contents of the control groups were 30% (Cu) respectively 30 Al 70 )、40％(Cu 40 Al 60 )、50％(Cu 50 Al 50 )、60％(Cu 40 Al 60 ) And 70% (Cu) 70 Al 30 ) The porosity of the copper-aluminum alloy sample after aluminum removal can be seen to be changed in a gradient manner along with the gradient change of the copper content.
4) Then, under the environment of dry vacuum, taking the porous copper obtained after dealloying as a carrier, taking mineral oil (MP 32 lubricating oil of American company) as lubricating oil, polishing the porous copper until the surface roughness Ra of the porous copper is about 0.5 mu m, and then ultrasonically cleaning the porous copper by acetone and drying the porous copper for later use; putting the porous copper-based bearing oil-free blank block into a beaker filled with a lubricant, putting the beaker into a vacuum drying oven, closing a cover of the vacuum oven at the set temperature of 40 ℃, opening a vacuumizing switch, vacuumizing to 0.09MPa of a pressure gauge, keeping for 30 minutes, then closing a vacuum pump, soaking the bearing material in the vacuum drying oven for 24 hours, soaking the liquid lubricant into the bearing pores, then closing the vacuum drying oven, naturally cooling to room temperature, deflating and opening the cover of the vacuum drying oven, taking out a sample, and wiping off the redundant lubricant on the surface by using oil absorption paper to obtain the organic/inorganic gradient composite material of the oil-containing bearing.
The oil-containing porous copper material is put into a centrifuge tube, and then a centrifugal test is carried out by using a high-speed centrifuge, the centrifugal rotating speed is 1000-4000r/m//, and 1000r/m//, is increased every 15 minutes. The centrifugal mass loss of the porous material at each rotation speed was calculated by measuring the mass of the lubricant-impregnated porous copper before and after the centrifugal experiment. The test results are shown in FIG. 7, and the results show that the oil content of the obtained organic/inorganic gradient composite material is 15.5%, and the oil retention rate after 4000r/m// centrifugation is 98.40%.
FIG. 8 is a graph of the coefficient of friction at load 6N rate of 200mm/m// reciprocating and the dry coefficient of friction without oil immersion after preparation of the gradient porous copper matrix impregnated slip agent PAO10 of example 1 of the present invention. The figure shows that: carrying out a reciprocating friction test under a dry friction test condition, wherein the average dry friction coefficient of the sample is 0.459; the average friction coefficient of the oil-containing composite material in a reciprocating oil-containing friction test is 0.123, and the oil-containing composite material has no large fluctuation in a long-time test process, which shows that the lubricating property is good.
Example 2
Provided is a method for preparing an organic/inorganic gradient composite material for an oil-impregnated bearing, comprising the steps of:
1) weighing copper powder and iron powder with the purity of more than or equal to 99.0 percent and the particle size of 0.2-5 mu m according to the atomic ratio of 60:40, 50:50 and 40:60, and ball-milling the mixed raw material powder on a light low-energy ball mill for 24 hours at the speed of 240 revolutions per minute to uniformly mix the composite powder;
2) and (2) filling the composite powder into a graphite mold by adopting a layering method, prepressing the sample for 10 minutes under the pressure of 5MPa, and then performing Plasma Activated Sintering (PAS), wherein the vacuum degree is less than or equal to 10Pa, the sintering temperature is 1000 ℃, the heating rate is 50 ℃/m//, the heat preservation time is 10m//, and the sintering pressure is 50MPa, so as to obtain the copper-aluminum alloy block.
3) Clean alloy is put into 5 wt% H 2 SO 4 The container was placed in a constant temperature water bath (90 ℃) and the time was recorded. Observing bubbles generated by the reaction of the active metal aluminum in the container and the sulfuric acid solution, finding that no bubbles are generated in the solution after 48 hours, then taking out the metal block, and repeatedly washing the metal block by using alcohol and deionized water. The obtained porous metal is a pure copper phase measured by an XRD method,the porosity of the obtained porous metal reaches 61.62%, the pore size distribution is within the range of 1-10 μm, and the compressive strength is 52.16 MPa.
4) Then, under the environment of dry vacuum, taking the porous copper obtained after dealloying as a carrier, taking mineral oil (MP 32 lubricating oil of American company) as lubricating oil, polishing the porous copper until the surface roughness Ra of the porous copper is about 0.5 mu m, and then ultrasonically cleaning the porous copper by acetone and drying the porous copper for later use; putting the porous copper-based bearing oilless blank block into a beaker filled with a lubricant, putting the beaker into a vacuum drying oven, closing a cover of the vacuum oven at the set temperature of 40 ℃, opening a vacuum switch, pumping to a pressure gauge of 0.09MPa, keeping for 30 minutes, then closing a vacuum pump, soaking the bearing material in the vacuum drying oven for 24 hours, soaking the liquid lubricant into the bearing pores, then closing the vacuum drying oven, naturally cooling to room temperature, deflating and opening the cover of the vacuum drying oven, taking out a sample, wiping off the redundant lubricant on the surface by using oil absorption paper, and obtaining the organic/inorganic gradient composite material of the oilbearing.
The oil-containing porous copper material is put into a centrifuge tube, and then a centrifugal test is carried out by using a high-speed centrifuge, the centrifugal rotating speed is 1000-4000r/m//, and 1000r/m//, is increased every 15 minutes. The mass of the porous copper impregnated with the lubricant before and after the centrifugal test was measured to calculate the centrifugal mass loss of the porous material at each rotation speed. The results showed that the oil content of the obtained organic/inorganic gradient composite material was 23.9% and the oil retention after 4000r/m// centrifugation was 95.3%.
Example 3
Provided is a method for preparing an organic/inorganic gradient composite material for an oil-impregnated bearing, comprising the steps of:
1) weighing copper powder and aluminum powder with the purity of more than or equal to 99.0 percent and the particle size of 0.2-5 mu m according to the atomic ratio of 60:40, 50:50 and 40:60, and ball-milling the mixed raw material powder on a light low-energy ball mill for 24 hours at the speed of 240 revolutions per minute to uniformly mix the composite powder;
2) and (2) filling the composite powder into a graphite mold by adopting a layering method, prepressing the sample for 10 minutes under the pressure of 5MPa, and then performing Plasma Activated Sintering (PAS), wherein the vacuum degree is less than or equal to 10Pa, the sintering temperature is 500 ℃, the heating rate is 50 ℃/m//, the heat preservation time is 10 minutes, and the sintering pressure is 50MPa, so that the copper-aluminum alloy block is obtained.
3) The cleaned alloy was placed in a 1mol/L hydrochloric acid solution and the container was placed in a constant temperature water bath (90 ℃ C.) and the time was recorded. Observing bubbles generated by the reaction of the active metal aluminum in the container and the sulfuric acid solution, finding that no bubbles are generated in the solution after 48 hours, then taking out the metal block, and repeatedly washing the metal block by using alcohol and deionized water. The obtained porous metal is pure copper phase, the porosity of the obtained porous metal reaches 64.13%, the pore size distribution is in the range of 0.1-0.3 μm, and the compressive strength is 48.31 MPa.
4) Then under the environment of dry vacuum, taking the porous copper obtained after dealloying as a carrier and polyolefin (PAO10) as lubricating oil, polishing the porous copper until the surface roughness Ra of the porous copper is about 0.5 mu m, and then ultrasonically cleaning the porous copper by acetone and drying the porous copper for later use; putting the porous copper-based bearing oil-free blank block into a beaker filled with a lubricant, putting the beaker into a vacuum drying oven, closing a cover of the vacuum oven at the set temperature of 150 ℃, opening a vacuumizing switch, vacuumizing to 0.09MPa of a pressure gauge, keeping for 30 minutes, then closing a vacuum pump, soaking the bearing material in the vacuum drying oven for 2 hours, soaking the liquid lubricant into the bearing pores, then closing the vacuum drying oven, naturally cooling to room temperature, deflating and opening the cover of the vacuum drying oven, taking out a sample, and wiping off the redundant lubricant on the surface by using oil absorption paper to obtain the organic/inorganic gradient composite material of the oil-containing bearing.
The oil-containing porous copper material is put into a centrifuge tube, and then a centrifugal test is carried out by using a high-speed centrifuge, the centrifugal rotating speed is 1000-4000r/m//, and 1000r/m//, is increased every 15 minutes. The centrifugal mass loss of the porous material at each rotation speed was calculated by measuring the mass of the lubricant-impregnated porous copper before and after the centrifugal experiment. The results showed that the oil content of the obtained organic/inorganic gradient composite material was 16.2% and the oil retention after 4000r/m// centrifugation was 97.40%.
Example 4
Provided is a method for preparing an organic/inorganic gradient composite material for an oil-impregnated bearing, comprising the steps of:
1) weighing copper powder and aluminum powder with the purity of more than or equal to 99.0 percent and the particle size of 0.2-5 mu m according to the atomic ratio of 60:40, 50:50, 40:60 and 0:100, and ball-milling the mixed raw material powder on a light low-energy ball mill at the speed of 240 r/min for 24 hours to uniformly mix the composite powder;
2) and (2) filling the composite powder into a graphite mold by adopting a layering method, prepressing the sample for 10 minutes under the pressure of 5MPa, and then performing Plasma Activated Sintering (PAS), wherein the vacuum degree is less than or equal to 10Pa, the sintering temperature is 500 ℃, the heating rate is 50 ℃/m//, the heat preservation time is 10 minutes, and the sintering pressure is 50MPa, so that the copper-aluminum alloy block is obtained.
3) The cleaned alloy was placed in a 10 wt% sulfuric acid solution and the container placed in a constant temperature water bath (90 ℃) and the time recorded. Observing bubbles generated by the reaction of the active metal aluminum in the container and the sulfuric acid solution, finding that no bubbles are generated in the solution after 36 hours, then taking out the metal block, and repeatedly washing the metal block by using alcohol and deionized water. The obtained porous metal is pure copper phase, the porosity of the obtained porous metal is 55.80%, the pore size distribution is in the range of 0.2-0.4 μm, and the compressive strength is 56.32 MPa.
4) Then under the environment of dry vacuum, taking the porous copper obtained after dealloying as a carrier and polyolefin (PAO10) as lubricating oil, polishing the porous copper until the surface roughness Ra of the porous copper is about 0.5 mu m, and then ultrasonically cleaning the porous copper by acetone and drying the porous copper for later use; putting the porous copper-based bearing oil-free blank block into a beaker filled with a lubricant, putting the beaker into a vacuum drying oven, closing a cover of the vacuum oven at the set temperature of 110 ℃, opening a vacuumizing switch, vacuumizing to 0.09MPa of a pressure gauge, keeping for 30 minutes, then closing a vacuum pump, soaking the bearing material in the vacuum drying oven for 3 hours to ensure that the liquid lubricant is soaked in the bearing pores, then closing the vacuum drying oven, naturally cooling to room temperature, deflating and opening the cover of the vacuum drying oven, taking out a sample, and wiping off the redundant lubricant on the surface by using oil absorption paper to obtain the organic/inorganic gradient composite material of the oil-containing bearing.
The oil-containing porous copper material is put into a centrifuge tube, and then a centrifugal test is carried out by using a high-speed centrifuge, the centrifugal rotating speed is 1000-4000r/m//, and 1000r/m//, is increased every 15 minutes. The centrifugal mass loss of the porous material at each rotation speed was calculated by measuring the mass of the lubricant-impregnated porous copper before and after the centrifugal experiment. The results showed that the oil content of the obtained organic/inorganic gradient composite material was 17.8% and the oil retention after 4000r/m// centrifugation was 98.10%.
Example 5
Provided is a method for preparing an organic/inorganic gradient composite material for an oil-impregnated bearing, comprising the steps of:
1) weighing copper powder and aluminum powder with the purity of more than or equal to 99.0 percent and the particle size of 0.2-5 mu m according to the atomic ratio of 60:40, 50:50 and 40:60, and ball-milling the mixed raw material powder on a light low-energy ball mill for 24 hours at the speed of 240 revolutions per minute to uniformly mix the composite powder; ,
2) and (2) filling the composite powder into a graphite mold by adopting a layering method, prepressing the sample for 10 minutes under the pressure of 5MPa, and then performing Plasma Activated Sintering (PAS), wherein the vacuum degree is less than or equal to 10Pa, the sintering temperature is 500 ℃, the heating rate is 50 ℃/m//, the heat preservation time is 10 minutes, and the sintering pressure is 50MPa, so that the copper-aluminum alloy block is obtained.
3) The cleaned alloy was placed in a 10 wt% sulfuric acid solution and the container was placed under a constant temperature water bath (90 ℃) and the time was recorded. Observing bubbles generated by the reaction of the active metal aluminum in the container and the sulfuric acid solution, finding that no bubbles are generated in the solution after 36 hours, then taking out the metal block, and repeatedly washing the metal block by using alcohol and deionized water. The obtained porous metal is a pure copper phase, the porosity of the obtained porous metal reaches 64.80 percent, the pore size distribution is in the range of 0.2-0.4 mu m, and the compressive strength is 46.32 MPa.
4) Then under the environment of dry vacuum, taking the porous copper obtained after dealloying as a carrier and polyolefin (PAO10) as lubricating oil, polishing the porous copper until the surface roughness Ra of the porous copper is about 0.5 mu m, and then ultrasonically cleaning the porous copper by acetone and drying the porous copper for later use; putting the porous copper-based bearing oilless blank block into a beaker filled with a lubricant, putting the beaker into a vacuum drying oven, closing a cover of the vacuum oven at the set temperature of 110 ℃, opening a vacuum switch, pumping to a pressure gauge of 0.09MPa, keeping for 30 minutes, then closing a vacuum pump, soaking the bearing material in the vacuum drying oven for 3 hours to ensure that the liquid lubricant is soaked in bearing pores, then closing the vacuum drying oven, naturally cooling to room temperature, deflating and opening the cover of the vacuum drying oven, taking out a sample, wiping off the redundant lubricant on the surface by using oil absorption paper, and obtaining the organic/inorganic gradient composite material of the oilbearing.
The oil-containing porous copper material is put into a centrifuge tube, and then a centrifugal test is carried out by using a high-speed centrifuge, the centrifugal rotating speed is 1000-4000r/m//, and 1000r/m//, is increased every 15 minutes. The centrifugal mass loss of the porous material at each rotation speed was calculated by measuring the mass of the lubricant-impregnated porous copper before and after the centrifugal experiment. The results showed that the oil content of the obtained organic/inorganic gradient composite material was 16.8% and the oil retention after 4000r/m// centrifugation was 97.10%.
Example 6
Provided is a method for preparing an organic/inorganic gradient composite material for an oil-impregnated bearing, comprising the steps of:
1) weighing copper powder and aluminum powder with the purity of more than or equal to 99.0 percent and the particle size of 0.2-5 mu m according to the atomic ratio of 100:0, 60:40, 50:50 and 40:60, and ball-milling the mixed raw material powder on a light low-energy ball mill at the speed of 240 r/min for 24 hours to uniformly mix the composite powder;
2) and (2) filling the composite powder into a graphite mold by adopting a layering method, prepressing the sample for 10 minutes under the pressure of 5MPa, and then performing Plasma Activated Sintering (PAS), wherein the vacuum degree is less than or equal to 10Pa, the sintering temperature is 500 ℃, the heating rate is 50 ℃/m//, the heat preservation time is 10 minutes, and the sintering pressure is 50MPa, so that the copper-aluminum alloy block is obtained.
3) The cleaned alloy was placed in a 10 wt% sulfuric acid solution and the container was placed under a constant temperature water bath (90 ℃) and the time was recorded. Observing bubbles generated by the reaction of the active metal aluminum in the container and the sulfuric acid solution, finding that no bubbles are generated in the solution after 36 hours, then taking out the metal block, and repeatedly washing the metal block by using alcohol and deionized water. The obtained porous metal is pure copper phase, the porosity of the obtained porous metal reaches 66.45%, the pore size distribution is in the range of 0.2-0.4 mu m, and the compressive strength is 49.32 MPa.
4) Then under the environment of dry vacuum, taking the porous copper obtained after dealloying as a carrier and polyolefin (PAO10) as lubricating oil, polishing the porous copper until the surface roughness Ra of the porous copper is about 0.5 mu m, and then ultrasonically cleaning the porous copper by acetone and drying the porous copper for later use; putting the porous copper-based bearing oil-free blank block into a beaker filled with a lubricant, putting the beaker into a vacuum drying oven, closing a cover of the vacuum oven at the set temperature of 110 ℃, opening a vacuumizing switch, vacuumizing to 0.09MPa of a pressure gauge, keeping for 30 minutes, then closing a vacuum pump, soaking the bearing material in the vacuum drying oven for 3 hours to ensure that the liquid lubricant is soaked in the bearing pores, then closing the vacuum drying oven, naturally cooling to room temperature, deflating and opening the cover of the vacuum drying oven, taking out a sample, and wiping off the redundant lubricant on the surface by using oil absorption paper to obtain the organic/inorganic gradient composite material of the oil-containing bearing.
The oil-containing porous copper material is put into a centrifuge tube, and then a centrifugal test is carried out by using a high-speed centrifuge, the centrifugal rotating speed is 1000-4000r/m//, and 1000r/m//, is increased every 15 minutes. The centrifugal mass loss of the porous material at each rotation speed was calculated by measuring the mass of the lubricant-impregnated porous copper before and after the centrifugal experiment. The results showed that the oil content of the obtained organic/inorganic gradient composite material was 15.8% and the oil retention after 4000r/m// centrifugation was 97.85%.
Example 7
A preparation method of an organic/inorganic gradient composite material for an oil-impregnated bearing is provided, which comprises the following steps:
1) weighing copper powder and iron powder with the purity of more than or equal to 99.0 percent and the particle size of 0.2-5 mu m according to the atomic ratio of 30:70, 25:75, 20:80 and 15:85, and ball-milling the mixed raw material powder on a light low-energy ball mill at the speed of 240 revolutions per minute for 24 hours to uniformly mix the composite powder;
2) and (2) filling the composite powder into a graphite mold by adopting a layering method, prepressing the sample for 10 minutes under the pressure of 5MPa, and then performing Plasma Activated Sintering (PAS), wherein the vacuum degree is less than or equal to 10Pa, the sintering temperature is 1000 ℃, the heating rate is 50 ℃/m//, the heat preservation time is 10 minutes, and the sintering pressure is 50MPa, so that the copper-aluminum alloy block is obtained.
3) Clean alloy is put into 5 wt% H 2 SO 4 The container was placed in a constant temperature water bath (90 ℃) and the time was recorded. Observing the bubbles of the reaction of the active metal aluminum and the sulfuric acid solution in the container, and finding out the solution after 48 hoursNo bubble is generated, and then the metal block is taken out and repeatedly washed by alcohol and deionized water. The obtained porous metal is pure copper phase, the porosity of the obtained porous metal is 58.62%, the pore size distribution is within the range of 1-10 μm, and the compressive strength is 54.16 MPa.
4) Then under the environment of dry vacuum, taking the porous copper obtained after dealloying as a carrier and polyolefin (PAO10) as lubricating oil, polishing the porous copper until the surface roughness Ra of the porous copper is about 0.5 mu m, and then ultrasonically cleaning the porous copper by acetone and drying the porous copper for later use; placing an oil-free blank block of the porous copper-based bearing into a beaker filled with a lubricant, placing the beaker into a vacuum drying oven, closing a cover of the vacuum oven at the set temperature of 100 ℃, opening a vacuum switch, pumping to a pressure gauge of 0.09Mpa, keeping for 30 minutes, then closing a vacuum pump, soaking the bearing material in the vacuum drying oven for 4 hours, soaking the liquid lubricant into the pores of the bearing, then closing the vacuum drying oven, naturally cooling to room temperature, deflating and opening the cover of the vacuum drying oven, taking out a sample, wiping off the redundant lubricant on the surface by using oil absorption paper, and thus obtaining the organic/inorganic gradient composite material of the oil-containing bearing.
The oil-containing porous copper material is put into a centrifuge tube, and then a centrifugal test is carried out by using a high-speed centrifuge, the centrifugal rotating speed is 1000-4000r/m//, and 1000r/m//, is increased every 15 minutes. The centrifugal mass loss of the porous material at each rotation speed was calculated by measuring the mass of the lubricant-impregnated porous copper before and after the centrifugal experiment. The results showed that the oil content of the obtained organic/inorganic gradient composite material was 34.3%, and the oil retention after 4000r/m// centrifugation was 97.3%.
Claims (10)
1. An organic/inorganic gradient composite material for an oil-impregnated bearing, comprising a gradient porous copper matrix and an organic lubricant impregnated in pores of the gradient porous copper matrix; wherein:
the gradient porous copper matrix is of a multilayer structure, and the porosity or pore diameter of each layer of porous copper is in gradient change.
2. The composite material of claim 1, wherein the porosity of each layer of porous copper in the gradient porous copper matrix varies in a gradient from 0% to 89.56%, and the pore size varies in a gradient from 0.1 μm to 10 μm.
3. The composite material of claim 1, wherein the organic lubricant is one or more of liquid paraffin, polyolefin, mineral oil, polyethylene glycol, polyalkyl cyclopentane, diester oil, and fully synthetic oil.
4. A method for preparing an organic/inorganic gradient composite for an oil-impregnated bearing according to any one of claims 1 to 3, comprising the steps of:
1) taking copper powder and active metal powder as raw materials, respectively weighing the copper powder and the active metal powder according to the designed layer number of each layer, and fully mixing, wherein the element content ratio of the copper powder and the active metal powder in the raw materials of each layer is changed in a gradient manner, and the active metal powder is one of aluminum powder and iron powder;
2) stacking each layer of raw material mixed powder obtained in the step 1), pressing and forming, preparing a copper alloy block by using a powder metallurgy technology, and removing active metal powder to prepare a gradient porous copper matrix;
3) soaking the gradient porous copper matrix obtained in the step 2) in an organic lubricant to enable the organic lubricant to be soaked in pores of the porous copper matrix, and obtaining the organic/inorganic gradient composite material for the oil-retaining bearing.
5. The method according to claim 4, wherein in step 1), the mass fraction of copper powder in each layer of raw material is not less than 10% and is varied in a gradient manner.
6. The preparation method according to claim 4, wherein in the step 2), the specific sintering process in the powder metallurgy technology is as follows: the heating rate is 50-200 ℃/m//, the sintering temperature is 400-.
7. The preparation method according to claim 4, wherein in the step 2), the step of removing the active metal powder comprises the following steps: and (3) putting the copper alloy block into a container filled with an acid solution, and reacting at a constant temperature until no bubbles are generated, thus obtaining the gradient porous copper matrix.
8. The production method according to claim 7, wherein the acid solution is a sulfuric acid solution; the constant temperature is 60-95 ℃.
9. The preparation method according to claim 4, wherein in the step 3), the gradient porous copper matrix is soaked in the organic lubricant under a vacuum drying condition, wherein the vacuum degree is more than or equal to 0.08 MPa; the soaking temperature is 40-150 ℃, and the soaking time is 2-24 hours.
10. The method according to claim 4, wherein in the step 3), the gradient porous copper matrix is polished to a surface roughness Ra ≦ 1 μm before being soaked in the organic lubricant.
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