CN117020196A - High-strength low-cost self-supplementing lubricating phase composite material and preparation method thereof - Google Patents
High-strength low-cost self-supplementing lubricating phase composite material and preparation method thereof Download PDFInfo
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- 230000001050 lubricating effect Effects 0.000 title claims abstract description 38
- 238000002360 preparation method Methods 0.000 title claims abstract description 21
- 239000000843 powder Substances 0.000 claims abstract description 140
- 229910052751 metal Inorganic materials 0.000 claims abstract description 8
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- 238000010438 heat treatment Methods 0.000 claims description 53
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- 238000002156 mixing Methods 0.000 claims description 22
- IMNFDUFMRHMDMM-UHFFFAOYSA-N N-Heptane Chemical group CCCCCCC IMNFDUFMRHMDMM-UHFFFAOYSA-N 0.000 claims description 21
- 238000000034 method Methods 0.000 claims description 19
- 238000000498 ball milling Methods 0.000 claims description 17
- 238000001816 cooling Methods 0.000 claims description 11
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 7
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- 229910002804 graphite Inorganic materials 0.000 claims description 7
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- 239000000203 mixture Substances 0.000 claims description 4
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- 238000003825 pressing Methods 0.000 claims description 2
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- 238000005461 lubrication Methods 0.000 abstract description 15
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- 229910017944 Ag—Cu Inorganic materials 0.000 description 1
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- CWQXQMHSOZUFJS-UHFFFAOYSA-N molybdenum disulfide Chemical compound S=[Mo]=S CWQXQMHSOZUFJS-UHFFFAOYSA-N 0.000 description 1
- 229910052982 molybdenum disulfide Inorganic materials 0.000 description 1
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- XOFYZVNMUHMLCC-ZPOLXVRWSA-N prednisone Chemical compound O=C1C=C[C@]2(C)[C@H]3C(=O)C[C@](C)([C@@](CC4)(O)C(=O)CO)[C@@H]4[C@@H]3CCC2=C1 XOFYZVNMUHMLCC-ZPOLXVRWSA-N 0.000 description 1
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Classifications
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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
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22C—FOUNDRY MOULDING
- B22C23/00—Tools; Devices not mentioned before for moulding
- B22C23/02—Devices for coating moulds or cores
-
- 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
- B22F3/02—Compacting only
- B22F3/03—Press-moulding apparatus therefor
-
- 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
-
- 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
-
- 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
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/24—After-treatment of workpieces or articles
- B22F2003/248—Thermal after-treatment
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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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- Engineering & Computer Science (AREA)
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- Manufacturing & Machinery (AREA)
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- Optics & Photonics (AREA)
- Powder Metallurgy (AREA)
Abstract
The invention belongs to the field of corrosion and self-lubrication, and in particular relates to a high-strength low-cost self-supplementing lubricating phase composite material and a preparation method thereof, wherein micron-sized Ti, ni or Co metal powder is used as base powder, the base powder is mixed with Mo powder, cu powder and Ag powder, the weight percentages of the base powder and the Mo powder are respectively 70-80%, 8-15%, 5-20% and 1-10%, and the particle sizes of original powder are respectively less than or equal to 20 microns, less than or equal to 10 microns, less than or equal to 53 microns and less than or equal to 53 microns. The composite material is compact and has no holes, high bending strength and compressive strength, excellent mechanical property, excellent self-lubricating property in a wide temperature range and good wear-resistant lubricating effect for a long time.
Description
Technical Field
The invention belongs to the field of corrosion and self-lubrication, and particularly relates to a high-strength low-cost self-supplementing lubricating phase composite material and a preparation method thereof.
Background
In the field of aerospace and other tip industries, the running environments of transmission moving parts with heavy-point types such as rotary seals, high-temperature bearings, bushings and the like are becoming severe. The synergistic coupling of high temperature corrosion and frictional wear has become a key factor affecting the reliability and life of the entire system as a main destructive mode of the material. According to statistics, the energy loss caused by the abrasion failure of the country can reach 30-50% of the total energy loss each year. In order to reduce the friction coefficient and wear rate between parts, lubricating oil and grease are usually added to the surfaces of the parts. However, in severe environments such as high temperature, high pressure, corrosion and the like, the lubricating oil and the lubricating grease fail, and the actual application requirements cannot be met. For some airtight or special parts, lubrication cannot be realized by adding solid lubricant. Therefore, metal powder is mixed with a solid lubricant, and then prepared into a metal-based self-lubricating composite material by a powder metallurgy method and processed into parts so as to meet the performance requirements of low friction coefficient and low wear rate.
The traditional self-lubricating material is prepared by compounding two or more solid lubricants, and the lubrication of the composite material in a wide temperature range is realized by utilizing the synergistic lubrication effect of a plurality of different lubricants at different temperatures. The self-lubrication is realized by means of soft metals such as Ag at room temperature to lower temperature, the content of the Ag must reach 15 wt percent or even 20 wt percent or more to realize the lubrication effect, and the high cost makes the application limited; the realization of high temperature self-lubrication depends on the addition of a large amount of fluoride, such as PS212 material developed by NASA, PS200 series thermal spraying coating material prepared by C Dellacort and the like, and Ni developed by Li Jianliang and the like 3 Al-W-Ag-fluoride composite material. The composite material or the coating material has excellent wide-temperature-range self-lubricating performance, but the ceramic phase introduced by a large amount of fluoride greatly reduces the fracture toughness, and the application of the composite material or the coating material in a high-load impact environment is limited. These factors cause severe bottlenecks in high temperature self-lubricating material design and application. How to make the lubricating material have self-lubrication, antifriction and wear resistanceThe anti-oxidation and other multiple functions, thereby improving the operation stability and the safety reliability of mechanical parts in severe service environments such as high vacuum degree, high radiation degree, high operation speed, high load, high temperature and the like, being free from the limitation of economic cost, being widely applied and becoming the main trend of the development of the current self-lubricating composite material.
In recent years, a high-temperature sweating self-compensating lubricating material is designed based on the synergistic principle of the wettability and the high-temperature lubricating performance of a lubricating body, such as Pb-Sn-Ag, pb-Sn-Ag-Cu lubricating materials developed by Yan Songshan and the like, and Pb-Sn-Ag-RE lubricating materials prepared by Zhang Guangming and the like. Adding the multi-element solid lubricating body into sweat gland type micropores of the porous metal ceramic matrix through an infiltration process to prepare the lubricating layer composite material with gradient distribution of lubricating elements, and realizing self-lubrication at high temperature by means of melting out of the low-melting-point lubricating body, namely high-temperature sweat-releasing lubrication of the alloy. The physical and chemical properties and the melting depth of the lubricating body determine the lubricating function and the lubricating service life of the composite material, and the melting of the lubricating body can lead to the poor wettability of the lubricating body and the metal ceramic matrix, so that the compactness and the mechanical property of the composite material are reduced. Therefore, the scheme of 'alloy sweating' cannot realize the coordination and optimization of the mechanical property and the self-lubricating property of the composite material. The previous work CN 113681009B discloses a self-supplementing lubricating phase composite material generated on a friction oxidation control surface and a preparation method thereof, and designs and prepares an Ag-containing composite material, wherein the Ag-containing composite material can balance mechanical properties and self-lubricating properties, but high-content Ag causes high economic cost and cannot be widely applied in a large range. Aiming at the difficult problems of mechanics, high-temperature oxidation and lubrication of high-temperature and load-bearing moving parts, development of a novel self-lubricating composite material with high strength, high toughness, excellent antifriction and wear resistance, high-temperature oxidation resistance and economy and universality is needed to be developed.
Disclosure of Invention
Aiming at the problems that the self-lubricating composite material in the prior art cannot fully have the functions of oxidation resistance, self-lubrication and high toughness, the economic limit is broken through, and the self-lubricating composite material can be used for large-scale production of motion and transmission parts under the conditions of oxidation resistance, high temperature resistance and high load impact. The technical scheme of the invention is as follows:
the composite material is prepared by mixing micron-sized Ti, ni or Co metal powder serving as base powder with 70-80% of Mo powder, 8-15% of Cu powder and 1-10% of Ag powder in percentage by mass, wherein the particle size of the original powder is less than or equal to 20 mu m, less than or equal to 10 mu m, less than or equal to 53 mu m and less than or equal to 53 mu m.
Furthermore, the high-strength low-cost self-supplementing lubricating phase composite material can be used for replacing Mo powder with a combination of Mo powder and W powder in any proportion.
Further, the high-strength low-cost self-supplementing lubricating phase composite material has the performance indexes that: the reciprocating friction coefficient is less than or equal to 0.3 and the wear rate is less than or equal to 6 multiplied by 10 within the wide temperature range from room temperature to 700 DEG C - 5 mm 3 ·N -1 ·m -1 The yield strength is more than or equal to 900 MPa, the crushing strength is more than or equal to 1850 MPa or no crushing.
The preparation method of the high-strength low-cost self-supplementing lubricating phase composite material comprises the following steps of:
(1) Powder mixing: mixing the powder raw materials weighed according to the formula by using a ball mill, stopping for 15-30 min every 30 min running at the rotating speed of 300-400 r/min, and drying the obtained uniform alloyed powder after the ball milling time is 15-40 h;
(2) And (3) die filling and cold pressing: uniformly spraying boron nitride on the inner wall of a die for sintering, filling graphite paper in the die, filling the alloyed powder obtained in the step (1) into the die, and prepressing the powder by using an oil press and keeping the powder at 60-120 s; pressurizing and maintaining for 2-3 min by using a universal tester, and unloading;
(3) Discharge plasma sintering: the prepared green body is pressed and sintered according to the process of heating I-heating II-heat preservation-cooling, and the vacuum degree is higher than 1 multiplied by 10 -3 The sintering pressure is 35-50 Mpa;
(4) And (3) carrying out muffle furnace heat treatment: and (3) placing the block obtained in the step (3) in a muffle furnace for heat treatment, and then air-cooling to room temperature.
According to the preparation method of the self-supplementing lubricating phase composite material with high strength and low cost, the ball mill used in the step (1) is a planetary ball mill, the ball mill tank is a stainless steel ball mill tank, the mixing balls are clean stainless steel balls with the total mass of 10 times of the mixture, and the ball mill auxiliary agent is n-heptane with the mass fraction of 2-6%.
Further, in the preparation method of the high-strength low-cost self-supplementing lubricating phase composite material, the prepressing condition of the oil press on the powder in the step (2) is 20-30 MPa and is kept above 60 s; and pressurizing to 70-80 kN by using a universal tester device in a mode of firstly quick-acting and then uniform-acting, and then unloading after 2-3 min.
Further, in the preparation method of the high-strength low-cost self-supplementing lubricating phase composite material, the highest temperature in the heating I stage in the step (3) is 800-1100 ℃, and the heating speed is 50-60 ℃/min; the highest temperature in the heating stage II is 900-1200 ℃, and the heating speed is 30-60 ℃/min; preserving heat for 10-20 min at the final sintering temperature of 900-1200 ℃ and then gradually cooling along with a furnace; the density of the sintered composite material is more than 98 percent.
Further, in the preparation method of the high-strength low-cost self-supplementing lubricating phase composite material, in the step (4), the heat treatment condition of the muffle furnace on the block is that the temperature is kept for 30-300 min in the air atmosphere at 700-800 ℃.
The invention has the advantages and beneficial effects that:
(1) The design idea of the invention is as follows: the micron-sized Ti or Ni or Co and the added alloy element Mo/W ensure the high-temperature strength of the alloy; the selective oxidation of Mo/W powder and the combination of the Mo/W powder with Cu powder and Ag powder during high-temperature friction wear induce the formation of low-melting-point composite oxide, so that sweating is caused, the effects of antifriction, friction reduction and self lubrication are achieved, and the defect that the toughness of composite materials is reduced by adding excessive self-lubricating ceramic phases such as fluoride, boron nitride and molybdenum disulfide in the traditional method is avoided; and the low-cost Cu is used for replacing Ag noble metal to optimize the components of the composite material, so that the preparation cost is greatly reduced, and the composite material can be applied on a large scale. The composite material has excellent comprehensive properties such as high strength, high toughness, oxidation resistance, high-temperature self-lubrication and the like;
(2) The composite material has simple preparation process, and the raw materials required by the formula can be directly purchased in the market;
(3) The composite material has low preparation cost and can be applied in a large range;
(4) The composite material is compact and has no holes, high bending strength and compressive strength and excellent mechanical property;
(5) The composite material has excellent self-lubricating performance in a wide temperature range, and can provide good wear-resistant lubricating effect for a long time;
(6) The composite material has good high-temperature performance and processability, good electric and heat conductivity and easy processing into hot end parts with various shapes and sizes.
Drawings
FIG. 1 (a) is a diagram of the structure of a composite material according to the present invention;
FIG. 1 (b) is a wear scar of the composite of the present invention at room temperature by a reciprocating frictional wear apparatus;
FIG. 2 (a) shows the surface texture of the composite material after oxidation at 700℃for 60 min in a muffle furnace apparatus;
FIG. 2 (b) shows the wear scar of the composite material subjected to high temperature oxidation control at room temperature by a reciprocating frictional wear apparatus.
Detailed Description
The following detailed description of specific embodiments of the invention is provided in connection with the accompanying drawings and examples which are set forth in a manner that illustrates, but are not intended to limit, the scope of the invention.
Example 1
In this embodiment, the composite material is prepared by mixing micron-sized Ti powder with Mo powder, cu powder and Ag powder, wherein the grain size of Ti powder is 10 μm, the grain size of Mo powder is about 4 μm, the grain size of Cu powder and Ag powder is about 30 μm, and the specific preparation parameters are as follows:
powder mixing: the composite material comprises the following components of 70 percent wt percent of Ti powder, 10 percent wt percent of Mo powder, 10 percent wt percent of Cu powder and 10 percent wt percent of Ag powder; ball milling and mixing by a planetary ball mill, taking 5% of n-heptane as a ball milling auxiliary agent, and drying the obtained uniform alloyed powder after the ball milling time is 16 h after the operation is stopped for 20 min every 30 min at the rotating speed of 320 r/min.
Discharge plasma sintering: putting the ball-milled mixed composite powder into a graphite mold, compacting, and carrying out pressurized sintering by a discharge plasma device according to the process of heating I-heating II-heat preservation-cooling, wherein the process parameters are as follows: vacuum degree 1X 10 -3 an atm; sintering pressure is 40 MPa; the sintering temperature in the heating I stage is 900 ℃, and the heating speed is 55 ℃/min; the sintering temperature of the 'heating II' stage is 1000 ℃, and the heating speed is 45 ℃/min; the incubation time was 15 min.
And (3) carrying out muffle furnace heat treatment: the composite material was kept at a constant temperature in an air atmosphere at 700 ℃ for 60 min, and then slowly cooled to room temperature in air.
The performance indexes of the composite material are as follows: the density is 98.9%; the yield strength is 1290 MPa, the compression strength is more than or equal to 1960 MPa, and the steel is not crushed.
The friction and wear test conditions are that the load is 10N and the diameter is 9.525 mm of Si 3 N 4 The ball was rubbed back and forth for 30 min at a linear velocity of 0.024, 0.024 m/s. Friction is carried out in the temperature range from room temperature to 700 ℃, the average friction coefficient is less than or equal to 0.26, and the average wear rate is less than or equal to 4.9x10 -5 mm 3 ·N -1 ·m -1 。
Example 2
In this embodiment, the composite material is prepared by mixing micron-sized Ni powder with a granularity of 10 μm, mo powder, cu powder and Ag powder, wherein the granularity of Ni powder is 10 μm, the granularity of Mo powder is about 4 μm, the granularity of Cu powder and Ag powder is about 15 μm, and the specific preparation parameters are as follows:
powder mixing: the composite material comprises 75% wt% of Ni powder, 10% wt% of Mo powder, 10% wt% of Cu powder and 5% wt% of Ag powder; ball milling and mixing by a planetary ball mill, taking 5% of n-heptane as a ball milling auxiliary agent, and drying the obtained uniform alloyed powder after the ball milling time is 16 h after the operation is stopped for 20 min every 30 min at the rotating speed of 320 r/min.
Discharge plasma sintering: putting the ball-milled mixed composite powder into a graphite mold, compacting, and performing discharge plasmaThe sub-equipment is pressed and sintered according to the process of heating I, heating II, heat preservation and cooling, and the technological parameters are as follows: vacuum degree 1X 10 -3 an atm; the sintering pressure is 45 MPa; the highest temperature in the heating I stage is 1050 ℃, and the heating speed is 55 ℃/min; the highest temperature of the 'heating II' stage is 1150 ℃, and the heating speed is 35 ℃/min; the incubation time was 15 min.
And (3) carrying out muffle furnace heat treatment: the composite material was kept at a constant temperature for 120 min in an air atmosphere at 700 c and then slowly cooled to room temperature in air.
The performance indexes of the composite material are as follows: the density is 99.2%; the yield strength is 908 MPa, the compression strength is more than or equal to 2000 MPa, and the steel is not crushed.
The friction and wear test conditions are that the load is 10N and the diameter is 9.525 mm of Si 3 N 4 The ball was rubbed back and forth for 30 min at a linear velocity of 0.024, 0.024 m/s. Friction is carried out at the temperature ranging from room temperature to 700 ℃, the average friction coefficient is less than or equal to 0.28, and the average wear rate is less than or equal to 5 multiplied by 10 -5 mm 3 ·N -1 ·m -1 。
Example 3
In the embodiment, micron-sized NiCr powder is taken as a base, the granularity is 10 mu m, and the composite material is prepared by mixing the composite material with Mo powder, cu powder and Ag powder, wherein the granularity of the NiCr powder is 10 mu m, the granularity of the Mo powder is about 4 mu m, the granularity of the Cu powder and the granularity of the Ag powder are about 15 mu m, and the specific preparation parameters are as follows:
powder mixing: the composite material comprises 73 percent wt percent of NiCr powder, 11 percent wt percent of Mo powder, 12 percent wt percent of Cu powder and 4 percent wt percent of Ag powder; ball milling and mixing by a planetary ball mill, taking 5% of n-heptane as a ball milling auxiliary agent, and drying the obtained uniform alloyed powder after the ball milling time is 20 h, wherein the rotating speed is 350 r/min and the stop time is 30 min each time of operation for 30 min.
Discharge plasma sintering: putting the ball-milled mixed composite powder into a graphite mold, compacting, and carrying out pressurized sintering by a discharge plasma device according to the process of heating I-heating II-heat preservation-cooling, wherein the process parameters are as follows: vacuum degree 1X 10 -3 an atm; sintering temperature of the sintering pressure 40 MPa in the heating I stage is 1100 ℃, and heating speed is 55 ℃/min; "heating II" stageThe sintering temperature of the section is 1200 ℃, and the heating speed is 35 ℃/min; the incubation time was 15 min.
And (3) carrying out muffle furnace heat treatment: the composite material was kept at a constant temperature for 120 min in an air atmosphere at 800 ℃, and then slowly cooled to room temperature in air.
The performance indexes of the composite material are as follows: the density is 99.5%; yield strength 985 MPa, compression strength 2010 MPa, and crushing.
The friction and wear test conditions are that the load is 10N and the diameter is 9.525 mm of Si 3 N 4 The ball was rubbed back and forth for 30 min at a linear velocity of 0.024, 0.024 m/s. Friction is carried out at the temperature ranging from room temperature to 800 ℃, the average friction coefficient is less than or equal to 0.22, and the average wear rate is less than or equal to 4.5x10 -5 mm 3 ·N -1 ·m -1 。
Example 4
In the embodiment, micron-sized Co powder is taken as a base, the granularity is 10 mu m, and the composite material is prepared by mixing the Co powder, the Mo powder, the Cu powder and the Ag powder, wherein the granularity of the Co powder is 10 mu m, the granularity of the Mo powder is about 4 mu m, the granularity of the Cu powder and the granularity of the Ag powder are about 5 mu m, and the specific preparation parameters are as follows:
powder mixing: the composite material comprises the following components of 74 percent wt percent of Co powder, 12 percent wt percent of Mo powder, 10 percent wt percent of Cu powder and 4 percent wt percent of Ag powder; ball milling and mixing by a planetary ball mill, taking 5% of n-heptane as a ball milling auxiliary agent, stopping for 15 min every 30 min of running at the rotating speed of 300 r/min, and drying the obtained uniform alloyed powder after the ball milling time is 16 h.
Discharge plasma sintering: putting the ball-milled mixed composite powder into a graphite mold, compacting, and carrying out pressurized sintering by a discharge plasma device according to the process of heating I-heating II-heat preservation-cooling, wherein the process parameters are as follows: vacuum degree 1X 10 -3 an atm; sintering pressure is 40 MPa; the sintering temperature in the heating I stage is 1050 ℃, and the heating speed is 55 ℃/min; the sintering temperature of the 'heating II' stage is 1150 ℃, and the heating speed is 35 ℃/min; the incubation time was 15 min.
And (3) carrying out muffle furnace heat treatment: the composite material was kept at a constant temperature in an air atmosphere at 700 ℃ for 150 min, and then slowly cooled to room temperature in air.
The performance indexes of the composite material are as follows: the compactness is 99.6 percent, the yield strength is 925 MPa, the compression strength is 2020 MPa, and the crushing is realized.
The friction and wear test conditions are that the load is 10N and the diameter is 9.525 mm of Si 3 N 4 The ball was rubbed back and forth for 30 min at a linear velocity of 0.024, 0.024 m/s. Friction is carried out at the temperature ranging from room temperature to 700 ℃, the average friction coefficient is less than or equal to 0.28, and the average wear rate is less than or equal to 4.8x10 -5 mm 3 ·N -1 ·m -1 。
Example 5
In the embodiment, micron-sized Co-based high-entropy alloy powder is taken as basic powder, the granularity is 10 mu m, and the composite material is prepared by mixing the Co-based high-entropy alloy powder with Mo powder, cu powder and Ag powder, wherein the granularity of the Co-based high-entropy alloy powder is 10 mu m, the granularity of the Mo powder is about 4 mu m, the granularity of the Cu powder and the granularity of the Ag powder are about 5 mu m, and the specific preparation parameters are as follows:
powder mixing: the composite material comprises 75 percent wt percent of Co-based high-entropy alloy powder, 10 percent wt percent of Mo powder, 10 percent wt percent of Cu powder and 5 percent wt percent of Ag powder according to the following component proportions; ball milling and mixing by a planetary ball mill, taking 5% of n-heptane as a ball milling auxiliary agent, stopping for 15 min every 30 min of running at the rotating speed of 300 r/min, and drying the obtained uniform alloyed powder after the ball milling time is 16 h.
Discharge plasma sintering: putting the ball-milled mixed composite powder into a graphite mold, compacting, and carrying out pressurized sintering by a discharge plasma device according to a process of heating I-heating II-heat preservation-cooling, wherein the sintering parameters are as follows: vacuum degree 1X 10 -3 an atm; sintering pressure is 40 MPa; the sintering temperature in the heating I stage is 1150 ℃, and the heating speed is 55 ℃/min; sintering temperature of 'heating II' stage is 1200 ℃, heating speed is 35 ℃/min; the incubation time was 15 min.
And (3) carrying out muffle furnace heat treatment: the composite material was kept at a constant temperature in an air atmosphere at 800 ℃ for 60 min, and then slowly cooled to room temperature in air.
The performance indexes of the composite material are as follows: the density is 99.6%; the yield strength is 1050 MPa, the compression strength is 2100 MPa, and the crushing is carried out.
The friction and wear test conditions are that the load is 10N and the diameter is 9.525 mm of Si 3 N 4 The ball was rubbed back and forth for 30 min at a linear velocity of 0.024, 0.024 m/s. Friction is carried out in the temperature range from room temperature to 700 ℃, the average friction coefficient is less than or equal to 0.21, and the average wear rate is less than or equal to 4.8x10 -5 mm 3 ·N -1 ·m -1 。
Comparative example 1
The difference from example 1 is that: the composite material comprises 75% wt% of Ti powder, 10% wt% of Mo powder, 10% wt% of Cu powder and 5% wt% of Ag powder.
The compactness of the composite material is 98.5%, the yield strength is 1450 MPa, the compression strength is more than or equal to 2000 MPa, the composite material is not crushed, the composite material rubs in the temperature range from room temperature to 700 ℃, the average friction coefficient is less than or equal to 0.30, and the average wear rate is less than or equal to 3.7X10 - 5 mm 3 ·N -1 ·m -1 . As shown in the figure 1 (a), the prepared composite material has compact internal structure and no obvious defects such as holes; the room temperature wear scar morphology is shown in fig. 1 (b), the surface does not form a continuous enamel layer, and a large number of obvious defects such as furrows are visible. Fig. 2 (a) shows the surface morphology of a composite material subjected to high temperature oxidation control, covered with a large amount of oxide. The room temperature wear scar morphology is shown in fig. 2 (b), where a smooth continuous and flat enamel layer is seen.
Comparative example 2
The difference from example 1 is that: the composite material comprises 60 percent wt percent of Ti powder, 10 percent wt percent of Mo powder, 10 percent wt percent of Cu powder and 20 percent wt percent of Ag powder.
The compactness of the composite material is 99.6%, the yield strength is 820 MPa, the compression strength is more than or equal to 1450 MPa, the composite material is not crushed, the average friction coefficient in the temperature range from room temperature to 700 ℃ is less than or equal to 0.20, and the high-temperature wear rate at 700 ℃ reaches 3.0 multiplied by 10 - 4 mm 3 ·N -1 ·m -1 。
Comparative example 3
The difference from example 1 is that: the composite material is prepared by replacing Mo powder with W powder with equivalent granularity of 4 mu m, and replacing Ti powder with Co-based high-entropy alloy powder, wherein the component proportion is 75% wt% of Co-based high-entropy alloy powder, 10% wt% of W powder, 10% wt% of Cu powder and 5% wt% of Ag powder.
The average friction coefficient of the composite material in the temperature range from room temperature to 700 ℃ is less than or equal to 0.23, and the composite material is flatThe average wear rate is less than or equal to 5 multiplied by 10 -5 mm 3 ·N -1 ·m -1 。
The applicant states that although the detailed composition and method of preparation of the present invention have been shown and described, it will be apparent to those skilled in the art that the present invention is not limited to practice with the aid of the detailed composition and method of preparation described above. Any improvement, substitution of product raw materials, addition of auxiliary components and the like of the invention are within the protection scope and the disclosure scope of the invention.
Claims (8)
1. The self-supplementing lubricating phase composite material is characterized in that the composite material takes micron-sized Ti, ni or Co metal powder as base powder, is mixed with Mo powder, cu powder and Ag powder, and respectively accounts for 70-80%, 8-15%, 5-20% and 1-10% by mass percent, and the particle size of the original powder is respectively less than or equal to 20 mu m, less than or equal to 10 mu m, less than or equal to 53 mu m and less than or equal to 53 mu m.
2. The high-strength low-cost self-supplementing lubricating phase composite material according to claim 1, wherein the Mo powder can be replaced by a combination of Mo powder and W powder in any proportion.
3. The high strength low cost self-compensating lubricating phase composite material of claim 1, wherein said composite material has performance metrics of: the reciprocating friction coefficient is less than or equal to 0.3 and the wear rate is less than or equal to 6 multiplied by 10 within the wide temperature range from room temperature to 700 DEG C -5 mm 3 ·N -1 ·m -1 The yield strength is more than or equal to 900 MPa, the crushing strength is more than or equal to 1850 MPa or no crushing.
4. A method of preparing a high strength low cost self-supplementing lubricating phase composite material according to any one of claims 1 to 3, comprising the steps of:
(1) Powder mixing: mixing the powder raw materials weighed according to the formula by using a ball mill, stopping for 15-30 min every 30 min running at the rotating speed of 300-400 r/min, and drying the obtained uniform alloyed powder after the ball milling time is 15-40 h;
(2) And (3) die filling and cold pressing: uniformly spraying boron nitride on the inner wall of a die for sintering, filling graphite paper in the die, filling the alloyed powder obtained in the step (1) into the die, and prepressing the powder by using an oil press and keeping the powder at 60-120 s; pressurizing and maintaining for 2-3 min by using a universal tester, and unloading;
(3) Discharge plasma sintering: the prepared green body is pressed and sintered according to the process of heating I-heating II-heat preservation-cooling, and the vacuum degree is higher than 1 multiplied by 10 -3 The sintering pressure is 35-50 Mpa;
(4) And (3) carrying out muffle furnace heat treatment: and (3) placing the block obtained in the step (3) in a muffle furnace for heat treatment, and then air-cooling to room temperature.
5. The preparation method of the high-strength low-cost self-supplementing lubricating phase composite material is characterized in that the ball mill used in the step (1) is a planetary ball mill, the ball mill tank is a stainless steel ball mill tank, the mixing balls are clean stainless steel balls with the total mass of 10 times of the mixture, and the ball mill auxiliary agent is n-heptane with the mass fraction of 2-6%.
6. The method for preparing the high-strength low-cost self-supplementing lubricating phase composite material according to claim 4, wherein the prepressing condition of the oil press on powder in the step (2) is 20-30 MPa and is kept above 60 s; and pressurizing to 70-80 kN by using a universal tester device in a mode of firstly quick-acting and then uniform-acting, and then unloading after 2-3 min.
7. The method for preparing the high-strength low-cost self-supplementing lubricating phase composite material, which is characterized in that the highest temperature in the heating I stage in the step (3) is 800-1100 ℃, and the heating speed is 50-60 ℃/min; the highest temperature in the heating stage II is 900-1200 ℃, and the heating speed is 30-60 ℃/min; preserving heat for 10-20 min at the final sintering temperature of 900-1200 ℃ and then gradually cooling along with a furnace; the density of the sintered composite material is more than 99 percent.
8. The method for preparing the high-strength low-cost self-supplementing lubricating phase composite material according to claim 4, wherein the muffle furnace is used for carrying out heat treatment on the block in the step (4) and keeping the temperature at a constant temperature for 30-300 min in an air atmosphere with the temperature of 700-800 ℃.
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