CN102943224A - Copper alloy base self-lubricating composite material and preparation method thereof - Google Patents

Copper alloy base self-lubricating composite material and preparation method thereof Download PDF

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CN102943224A
CN102943224A CN201210503144XA CN201210503144A CN102943224A CN 102943224 A CN102943224 A CN 102943224A CN 201210503144X A CN201210503144X A CN 201210503144XA CN 201210503144 A CN201210503144 A CN 201210503144A CN 102943224 A CN102943224 A CN 102943224A
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carbon fiber
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CN102943224B (en
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陈岁元
刘常升
梁京
李新荣
安迪
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Northeastern University China
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Northeastern University China
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Abstract

The invention belongs to the technical field of materials, and particularly relates to a copper alloy base self-lubricating composite material and a preparation method thereof. The composite material comprises the following chemical components in percentage by mass: 9-10% of Ni, 0.5-1% of Sm2O3, 0.5-1% of MoS2, 0-1% of Ag, 0-2% of CaF2, 1-2% of Al2O3, 0-3% of W, 1-3% of nickel-plated graphite, 1.1-3.0% of copper-plated carbon fiber, 0-2.8% of pore forming agent NH4HCO3 and the balance of ZQSn663 tin bronze powder. The preparation method comprises the following steps: mixing the components, pressing to obtain a sample, sintering, performing hot dipping with composite PTFE (polytetrafluoroethylene), and drying to prepare the composite material. Through a method combining powder metallurgy sintering and composite hot dipping and hole sealing technologies, the novel copper alloy base composite self-lubricating material which has high strength, high wear resistance and self-lubricating property can be prepared in an environment-friendly and low-cost way. By regulating and controlling the components and technologies, the density of the prepared copper alloy base composite self-lubricating material is 4.71-6.54 g/cm<3>, the hardness is 30-58 HV, the crushing strength is 99-222 MPa, and the friction coefficient is 0.15-0.06, thereby meeting the requirements for self-lubricating materials of friction bushings under different working conditions.

Description

One Albatra metal-based self lubricated composite material and preparation method thereof
 
Technical field
The invention belongs to the material technology field, particularly Albatra metal-based self lubricated composite material and preparation method thereof.
Background technology
Friction parts occupies larger proportion in the mechanical means in the industrial structure, and socio-economic development is had larger impact, and lubricated in the friction parts working process is to improve part life, guarantee the key that mechanical means can normally be moved.Lubricated is the most effective measures of reducing friction, reduce wearing and tearing, general method is to use lubricating oil or lubricating grease, but at high temperature, vacuum, at a high speed, low speed, heavy duty, be difficult for forming under the abominable special operation condition conditions such as oil-bound film or oil film easily lost efficacy, component generally are difficult for adopting lubricating oil or lubricating grease to be lubricated.Along with the running speed of modern machines and mechanism and sharply increasing of load, and because make, the industries such as food, pharmacy are to the requirement of safety, health and anti-oil pollution, research and development have novel material and the technology of preparing thereof of high abrasion and self-lubricating property, have important using value with the development that adapts to relevant industries oil-free lubricatoin technology.
So far the copper alloy graphite composite material be widely used in making, the friction mechanical component axle sleeves such as food, pharmacy are with one of metal-based self-lubricating composite material, and the powder metallurgy technology of preparing is major techniques of preparation copper alloy foundation stone China ink self-lubricating composite because have the low and easy compound characteristics of cost.Yet prior powder metallurgy copper alloy graphite self-lubricating material is the same with general agglomerated material, low, the poor toughness of intensity, and after temperature was higher than 300 ℃, its matrix strength obviously descended, and wear resistance reduces.When it is used as self-lubricating composite, not only need high wear resisting property, and need to have excellent self-lubricating function concurrently, this need to carry out the mutually collaborative matching Design that forms of two aspects of metallic matrix and solid lubrication, in order to form the copper alloy base composite material of high-strength, high-anti-friction self-lubricating.Yet, powder metallurgy prepares between the high-wear resistance of material and the high self-lubricity energy and exists competitive relation, the raising that is high self-lubricating property is to be based upon on the basis of the ratio of solid lubrication phase in material increase, when improving the ratio of solid lubrication phase, tend to reduce the mechanical property of material, crushing strength, density and hardness are reduced, cause the wear resisting property of material to reduce.So the technology that low-cost preparation has the new copper alloy-based composite self-lubricating material of high abrasion is demanded development urgently.
In recent years because the fast development of nanotechnology and nano material, utilize the super lubricity that nano material has and strengthen the characteristics such as wear-resisting effect in conjunction with the characteristics of prior powder metallurgy technology of preparing, preparation has the matrix material of high abrasion and high lubricating property simultaneously, becomes the developing direction of technical study.
Summary of the invention
For deficiency of the prior art, the invention provides a kind of new copper alloy-based self-lubricating composite that has high abrasion and high self-lubricating property concurrently and preparation method thereof, purpose is to utilize the powder metallurgy technology of preparing, various one-tenth by material are grouped into the science design, the collaborative matching effect of performance copper alloy matrix, wild phase, solid lubrication phase and hole, research obtain to have oil-free lubricatoin friction parts new copper alloy-based self-lubricating composite and preparation modern technique thereof under the different application of the satisfying working condition.
An Albatra metal-based self lubricated composite material of the present invention, its chemical ingredients is by mass percentage: Ni 9 ~ 10%, Sm 2O 30.5 ~ 1%, MoS 20.5 ~ 1%, Ag 0 ~ 1%, CaF 20 ~ 2%, Al 2O 31 ~ 2%, W 0 ~ 3%, nickel plating graphite 1 ~ 3%, copper carbon fiber 1.1 ~ 3.0%, pore-forming material NH 4 HCO 30 ~ 2.8%, ZQSn663 tinbronze powder 73.7 ~ 81.5%, and its density is 4.71 ~ 6.54g/cm 3, hardness is 30 ~ 58HV, crushing strength 99 ~ 222MPa, frictional coefficient are 0.15 ~ 0.06.
Wherein, the chemical ingredients of described ZQSn663 tinbronze powder is Zn5 ~ 7% by mass percentage, Sn5 ~ 7%, and Pb2 ~ 4%, surplus is copper; Described copper carbon fiber diameter is 1 ~ 2 μ m, and length is 1 ~ 2mm.
The preparation method of an Albatra metal-based self lubricated composite material of the present invention may further comprise the steps:
(1) batch mixing: expect the mixing of powder with barrel at mixer, the mixer rotating speed is 300 ~ 400r/min, adds steel ball in the barrel and spring forms abrasive material, and making abrasive material and metallurgical volume ratio with composite powder is 7:1; Wherein metallurgy carries out according to the following steps with the composite powder batch mixing:
(a) take by weighing respectively Ni, Sm 2O 3, MoS 2, Ag, CaF 2, Al 2O 3, W, nickel plating graphite, copper carbon fiber, pore-forming material NH 4HCO 3Stand-by with ZQSn663 tinbronze powder, the amount of taking by weighing is Ni 9 ~ 10%, Sm by mass percentage 2O 30.5 ~ 1%, MoS 20.5 ~ 1%, Ag 0 ~ 1%, CaF 20 ~ 2%, Al 2O 31 ~ 2%, W 0 ~ 3%, nickel plating graphite 1 ~ 3%, copper carbon fiber 1.1 ~ 3.0%, pore-forming material NH 4HCO 30 ~ 2.8%, ZQSn663 tinbronze powder 73.7 ~ 81.5%;
The nanometer Al that (b) will take by weighing 2O 3Powder and ZQSn663 tinbronze powder be 1:1 wet mixing 5 ~ 8h in mass ratio, forms the master alloy powder;
The W powder that (c) will take by weighing and ZQSn663 tinbronze powder form the master alloy powder in mass ratio for 1:1 is dry mixed 5 ~ 8h;
(d) get the nanometer Al of step (b) 2O 3The W powder master alloy powder of master alloy powder and step (c) adds Ni, the Sm that takes by weighing again 2O 3, MoS 2, Ag, CaF 2, nickel plating graphite and remaining ZQSn663 tinbronze powder be dry mixed 6 ~ 8h, the compacting sample powder that evenly becomes to be mixed;
(e) get the copper carbon fiber that takes by weighing, being cut to the short carbon fiber that length is 1 ~ 2mm, is glycerine and the alcohol wiring solution-forming of 1:1 with volume ratio, with magnetic stirring apparatus the carbon fiber bubble is stirred 5 ~ 8h in solution, carbon fiber is spread out mutually, then clean with distilled water;
(f) powder that the copper carbon fiber of step (e) being handled well and step (d) mix is placed on and forms complex alloy powder in the container, adding quality is the binding agent Zinic stearas of complex alloy powder quality 0.5 ~ 1% again, add distilled water with its submergence, under electric mixer, stir 8h, the powder and the copper carbon fiber that stir are placed in the baking oven 80 ℃ of oven dry; Then the composite powder after will drying is put into ball mill again and is dry mixed 4 ~ 6h;
The pore-forming material NH that (g) will take by weighing 4HCO 3Be dry mixed 5 ~ 6h in the adding step (f), become the metallurgical composite powder of using;
(2) sample compacting: according to the loose density of powder and the sintered density weighing of setting, sample carry out Bidirectional pressure system at hydropress, guarantee in the pressing process to pressurize evenly, slowly and the release of pressure process, then reach pressurize 1min behind the predetermined pressing pressure 563MPa, so that gas can be discharged smoothly, guarantee that simultaneously powder fully tamps in die cavity;
(3) sintering of sample: the sample that suppresses is sintering under tube furnace hydrogen shield atmosphere, the sintering hydrogen pressure is 0.7 ~ 0.8MPa, be incubated 1h after being heated to 600 ℃ with the heat-up rate of 3 ℃/min, then be heated to 940 ℃ with the heat-up rate of 3 ℃/min and carry out heat preservation sintering 4h, then outage, under the condition of continuous protective atmosphere, be lower than 200 ℃ with the stove water cooling to the sample area temperature after sample come out of the stove;
(4) sample after sintering is finished carries out the compound PTFE of hot dipping: water-bath is heated to 50 ℃ ~ 70 ℃, again the sample that sinters is placed in the beaker that PTFE liquid is housed, beaker is put into water-bath hot dipping 1.5h, sample that hot dipping is good takes out, and is placed on that 120 ℃ of oven dry are prepared into matrix material in the drying baker; If the pore-forming material addition is 0, then need not carry out this step.
Characteristics of the present invention and beneficial effect are:
Principle of the present invention is to add Ni, W, nanometer Al from the design of material angle in copper alloy matrix 2O 3, carbon fiber, rare earth oxide etc. strengthen the wear resistance of matrix material, simultaneously, add nickel plating graphite, molybdenumdisulphide, Ag, CaF 2Improve mutually the self-lubricating property of material Deng solid lubrication, the one-tenth that forms science is grouped into, and under the powder metallurgy preparation technology who has optimized, prepares matrix material and porous sintered material with excellent mechanical performances and self-lubricating property.For porous sintered material, utilize the fluent material contain ultra-fine enhancing self-lubricating phase to carry out the sealing of hole consonance and process, the total content that obtains the solid lubrication phase reaches 30 ~ 40% the compound technology of preparing of novel material than high-wearing feature and better self-lubricating property of having.
The new copper alloy-based composite self-lubricating material that the method preparation that the inventive method can environmental protection, low cost utilizes powder metallurgy sintered and compound hot dipping hole sealing technology to combine has high strength, high abrasion and self-lubricating property.By composition and technical regulation, the density of the composite self-lubricating material of preparation reaches 4.71 ~ 6.74g/cm 3, hardness reaches 30 ~ 58HV, crushing strength 99 ~ 222MPa, frictional coefficient reaches 0.15 ~ 0.06 copper alloy base composite self-lubricating material, thereby satisfy under the different working conditions (such as high speed light loading, low-speed heave-load) to the demand of friction axle sleeve self-lubricating material.The advanced composite material of the present invention's preparation has high wear resisting property and good self-lubricating property concurrently, has important using value.
Description of drawings
Fig. 1 is sample sintering process graphic representation of the present invention;
Fig. 2 is the stereoscan photograph that contains 2.5wt.% copper carbon fiber composite sample of embodiment 5 preparations;
Fig. 3 is the 1.8wt.%NH that contains of embodiment 9 preparations 4HCO 3The scanning electron microscope shape appearance figure of composite sample;
Fig. 4 is for containing 1.8wt.%NH 4HCO 3The scanning shape appearance figure of composite sample composite sample behind 50 ℃ (a), 60 ℃ (b) and 70 ℃ (c) lower hot dipping PTFE;
Fig. 5 is the 1.8wt.%NH that contains of embodiment 9 preparations 4HCO 3The line sweep figure of composite sample sample behind 60 ℃ of lower hot dipping PTFE;
Fig. 6 is the 1.8wt.%NH that contains of embodiment 9 preparations 4HCO 3The X-ray diffraction analysis of composite sample sample behind 60 ℃ of lower hot dipping PTFE;
Fig. 7 is that sample is at 60 ℃ of lower hot dipping PTFE(a) and do not have hot dipping PTFE(b) frictional coefficient of composite sample changes comparison diagram in time;
Fig. 8 is that sample is at 60 ℃ of lower hot dipping PTFE(a) and do not have hot dipping PTFE(b) scanning shape appearance figure after the composite sample wearing and tearing.
Embodiment
The present invention will be further described below in conjunction with embodiment.
Density and porosity measurement are carried out according to standard GB/T 5123-1985 in the embodiment of the invention, scleroscopic instrument title model 450SVD Vickers' hardness instrument, the instrument title model LJ-3000A type mechanical type tensile testing machine of the routed intensity of pressure measurement, the instrument title model MG-2000 type high temperature friction and wear trier of survey frictional coefficient.
Embodiment 1
Prepare an Albatra metal-based self lubricated composite material, its chemical ingredients is Ni10%, Sm by mass percentage 2O 31%, MoS 21%, Ag1%, CaF 21%, Al 2O 32%, W3%, nickel plating graphite 3%, ZQSn663 tinbronze powder (chemical ingredients is Zn5% by mass percentage in the ZQSn663 tinbronze powder, Sn5%, Pb2%, copper 88%) 78%, its performance is as shown in table 1, and the preparation method is as follows:
(1) batch mixing: expect the mixing of powder with barrel at mixer, the mixer rotating speed is 400r/min, adds steel ball in the barrel and spring forms abrasive material, and making abrasive material and metallurgical volume ratio with composite powder is 7:1, is conducive to stirring and evenly mixes; Wherein metallurgy carries out according to the following steps with the composite powder batch mixing:
(a) take by weighing respectively Ni, Sm 2O 3, MoS 2, Ag, CaF 2, Al 2O 3, W, nickel plating graphite and ZQSn663 tinbronze powder be stand-by, the amount of taking by weighing is Ni10%, Sm by mass percentage 2O 31%, MoS 21%, Ag1%, CaF 21%, Al 2O 32%, W3%, nickel plating graphite 3%, ZQSn663 tinbronze powder 78%;
The nanometer Al that (b) will take by weighing 2O 3Powder and ZQSn663 bronze powder in mass ratio 1:1 are put into mixing tank, add an amount of dehydrated alcohol as grinding medium, put the mixing of rolling in the ball mill after the sealing into, take out behind the rotating speed 400r/min wet mixing 7h of ball mill, it is stand-by to form the master alloy powder behind drying at room temperature, fragmentation, mistake 200 mesh sieves;
The W powder that (c) will take by weighing and ZQSn663 bronze powder form the master alloy powder in mass ratio for 1:1 is dry mixed 6h;
(d) get the nanometer Al of step (b) 2O 3The W powder master alloy powder of master alloy powder and step (c) adds Ni, the Sm that takes by weighing again 2O 3, MoS 2, Ag, CaF 2, nickel plating graphite and remaining ZQSn663 tinbronze powder, be dry mixed 6h, the compacting sample powdered alloy that evenly becomes to be mixed; Adding quality is the binding agent Zinic stearas of complex alloy powder quality 0.5% again, add distilled water with its submergence, under electric mixer, stir 8h, the powder and the copper carbon fiber that stir are placed in the drying baker, 80 ℃ of oven dry 2h, the composite powder after then will drying is put into ball mill again and is dry mixed 4h;
(2) sample compacting: a, weighing: according to the loose density of powder and the sintered density weighing of setting; B, dress mould: in the powder mould of packing into gently with weighing, with suitable power knock and the method that shakes make powder in die cavity, be evenly distributed as far as possible, smooth, with carrying out smoothly of assurance binder process; C, compacting: carry out Bidirectional pressure system at hydropress, predetermined pressing force is 563MPa, and slowly operation guarantees certain volume under pressure, and overflows pressurize 1min when reaching 563MPa for the more all even hole Airs that make the pressure transmission have enough time; D, the demoulding: after removing pressure, will eject in the sample from mould with special-purpose push rod, to be sintered;
(3) sintering of sample: the sample that suppresses is sintering under tube furnace hydrogen shield atmosphere, and the sintering hydrogen pressure is 0.7 ~ 0.8MPa, and sample is placed in the stainless steel sintering boat, uses Al 2O 3After sand covers sample; push the burner hearth middle part; close fire door; plugged is incubated 1h after being heated to 600 ℃ with the heat-up rate of 3 ℃/min; allow Zinic stearas decompose gradually and volatilize; avoid sintered compact surface cracking, foaming, buckling deformation; heat-up rate with 3 ℃/min is heated to 940 ℃ of insulation 4h again; then outage; under the condition of continuous protective atmosphere; sample is slided into the furnace roof position of the cold inner cover of water in advance, and water flowing cools to furnace temperature displays temperature (the actual sample regional temperature is lower than 200 ℃) below 350 ℃ with the furnace, close hydrogen after sample come out of the stove.Fig. 1 is the sintering process graphic representation of sample.
Embodiment 2
Prepare an Albatra metal-based self lubricated composite material, its chemical ingredients is Ni10%, Sm by mass percentage 2O 31%, MoS 21%, Ag1%, CaF 21%, Al 2O 32%, (chemical ingredients is Zn5% by mass percentage in the ZQSn663 tinbronze powder for W 3%, nickel plating graphite 3%, copper carbon fiber (diameter is 1 μ m) 1.1%, ZQSn663 tinbronze powder, Sn5%, Pb2%, copper 88%) 76.9%, its performance is as shown in table 1, and its preparation method is as follows:
(1) batch mixing: expect the mixing of powder with barrel at mixer, the mixer rotating speed is 400r/min, adds steel ball in the barrel and spring forms abrasive material, and making abrasive material and metallurgical volume ratio with composite powder is 7:1, is conducive to stirring and evenly mixes; Wherein metallurgy carries out according to the following steps with the composite powder batch mixing:
(a) take by weighing respectively Ni, Sm 2O 3, MoS 2, Ag, CaF 2, Al 2O 3, W, nickel plating graphite, copper carbon fiber and ZQSn663 tinbronze powder be stand-by, the amount of taking by weighing is Ni10%, Sm by mass percentage 2O 31%, MoS 21%, Ag1%, CaF 21%, Al 2O 32%, W 3%, nickel plating graphite 3%, copper carbon fiber 1.1%, ZQSn663 tinbronze powder 76.9%;
The nanometer Al that (b) will take by weighing 2O 3Powder and ZQSn663 bronze powder in mass ratio 1:1 are put into mixing tank, add an amount of dehydrated alcohol as grinding medium, put the mixing of rolling in the ball mill after the sealing into, take out behind the rotating speed 400r/min wet mixing 7h of ball mill, it is stand-by to form the master alloy powder behind drying at room temperature, fragmentation, mistake 200 mesh sieves;
The W powder that (c) will take by weighing and ZQSn663 bronze powder form the master alloy powder in mass ratio for 1:1 is dry mixed 6h;
(d) get the nanometer Al of step (b) 2O 3The W powder master alloy powder of master alloy powder and step (c) adds Ni, the Sm that takes by weighing again 2O 3, MoS 2, Ag, CaF 2, nickel plating graphite and remaining ZQSn663 tinbronze powder, be dry mixed 6h, the compacting sample powder that evenly becomes to be mixed;
(e) get the copper carbon fiber that takes by weighing, being cut to the short carbon fiber that length is 1mm, is glycerine and the alcohol wiring solution-forming of 1:1 with volume ratio, with magnetic stirring apparatus the carbon fiber bubble is stirred 8h in solution, carbon fiber is spread out mutually, then clean with distilled water;
(f) powder that the copper carbon fiber of step (e) being handled well and step (d) mix is placed on and forms complex alloy powder in the container, adding quality is the binding agent Zinic stearas of complex alloy powder quality 0.5% again, add distilled water with its submergence, under electric mixer, stir 8h, the powder and the copper carbon fiber that stir are placed in the drying baker, 80 ℃ of oven dry 2h, the composite powder after then will drying is put into ball mill again and is dry mixed 4h;
Step (2), step (3) are identical with step (2), the step (3) of embodiment 1.
Embodiment 3
Prepare an Albatra metal-based self lubricated composite material, its chemical ingredients is Ni10%, Sm by mass percentage 2O 31%, MoS 21%, Ag1%, CaF 21%, Al 2O 32%, (chemical ingredients is Zn5% by mass percentage in the ZQSn663 tinbronze powder for W 3%, nickel plating graphite 3%, copper carbon fiber (diameter is 1 μ m) 1.6%, ZQSn663 tinbronze powder, Sn5%, Pb2%, copper 88%) 76.4%, its performance is as shown in table 1, and the preparation method is as follows:
(1) batch mixing: expect the mixing of powder with barrel at mixer, the mixer rotating speed is 400r/min, adds steel ball in the barrel and spring forms abrasive material, and making abrasive material and metallurgical volume ratio with composite powder is 7:1, is conducive to stirring and evenly mixes; Wherein metallurgy carries out according to the following steps with the composite powder batch mixing:
(a) take by weighing respectively Ni, Sm 2O 3, MoS 2, Ag, CaF 2, Al 2O 3, W, nickel plating graphite, copper carbon fiber and ZQSn663 tinbronze powder be stand-by, the amount of taking by weighing is Ni10%, Sm by mass percentage 2O 31%, MoS 21%, Ag1%, CaF 21%, Al 2O 32%, W 3%, nickel plating graphite 3%, copper carbon fiber 2.0%, ZQSn663 tinbronze powder 76.4%;
The nanometer Al that (b) will take by weighing 2O 3Powder and ZQSn663 bronze powder are put into mixing tank for 1:1 in mass ratio, add an amount of dehydrated alcohol as grinding medium, put the mixing of rolling in the ball mill after the sealing into, take out behind the rotating speed 400r/min wet mixing 7h of ball mill, it is stand-by to form the master alloy powder behind drying at room temperature, fragmentation, mistake 200 mesh sieves;
The W powder that (c) will take by weighing and ZQSn663 bronze powder form the master alloy powder in mass ratio for 1:1 is dry mixed 6h;
(d) get the nanometer Al of step (b) 2O 3The W powder master alloy powder of master alloy powder and step (c) adds Ni, the Sm that takes by weighing again 2O 3, MoS 2, Ag, CaF 2, nickel plating graphite and remaining ZQSn663 tinbronze powder, be dry mixed 6h, the compacting sample powder that evenly becomes to be mixed;
(e) get the copper carbon fiber that takes by weighing, being cut to the short carbon fiber that length is 1mm, is glycerine and the alcohol wiring solution-forming of 1:1 with volume ratio, with magnetic stirring apparatus the carbon fiber bubble is stirred 8h in solution, carbon fiber is spread out mutually, then clean with distilled water;
(f) powder that the copper carbon fiber of step (e) being handled well and step (d) mix is placed on and forms complex alloy powder in the container, adding quality is the binding agent Zinic stearas of complex alloy powder quality 0.5% again, add distilled water with its submergence, under electric mixer, stir 8h, the powder and the copper carbon fiber that stir are placed in the drying baker, 80 ℃ of oven dry 2h, the composite powder after then will drying is put into ball mill again and is dry mixed 6h;
Step (2), step (3) are identical with step (2), the step (3) of embodiment 1.
Embodiment 4
Prepare an Albatra metal-based self lubricated composite material, its chemical ingredients is Ni10%, Sm by mass percentage 2O 31%, MoS 21%, Ag1%, CaF 21%, Al 2O 32%, (chemical ingredients is Zn5% by mass percentage in the ZQSn663 tinbronze powder for W 3%, nickel plating graphite 3%, copper carbon fiber (diameter is 1 μ m) 2.0%, ZQSn663 tinbronze powder, Sn5%, Pb2%, copper 88%) 76.0%, its performance is as shown in table 1, and the preparation method is as follows:
(1) batch mixing: expect the mixing of powder with barrel at mixer, the mixer rotating speed is 400r/min, adds steel ball in the barrel and spring forms abrasive material, and making abrasive material and metallurgical volume ratio with composite powder is 7:1, is conducive to stirring and evenly mixes; Wherein metallurgy carries out according to the following steps with the composite powder batch mixing:
(a) take by weighing respectively Ni, Sm 2O 3, MoS 2, Ag, CaF 2, Al 2O 3, W, nickel plating graphite, copper carbon fiber and ZQSn663 tinbronze powder be stand-by, the amount of taking by weighing is Ni10%, Sm by mass percentage 2O 31%, MoS 21%, Ag1%, CaF 21%, Al 2O 32%, W 3%, nickel plating graphite 3%, copper carbon fiber 2.5%, ZQSn663 tinbronze powder 76.0%;
The nanometer Al that (b) will take by weighing 2O 3Powder and ZQSn663 bronze powder are put into mixing tank for 1:1 in mass ratio, add an amount of dehydrated alcohol as grinding medium, put the mixing of rolling in the ball mill after the sealing into, take out behind the rotating speed 400r/min wet mixing 7h of ball mill, it is stand-by to form the master alloy powder behind drying at room temperature, fragmentation, mistake 200 mesh sieves;
The W powder that (c) will take by weighing and ZQSn663 bronze powder form the master alloy powder in mass ratio for 1:1 is dry mixed 6h;
(d) get the nanometer Al of step (b) 2O 3The W powder master alloy powder of master alloy powder and step (c) adds Ni, the Sm that takes by weighing again 2O 3, MoS 2, Ag, CaF 2, nickel plating graphite and remaining ZQSn663 tinbronze powder, be dry mixed 6h, the compacting sample powder that evenly becomes to be mixed;
(e) get the copper carbon fiber that takes by weighing, being cut to the short carbon fiber that length is 1mm, is glycerine and the alcohol wiring solution-forming of 1:1 with volume ratio, with magnetic stirring apparatus the carbon fiber bubble is stirred 8h in solution, carbon fiber is spread out mutually, then clean with distilled water;
(f) powder that the copper carbon fiber of step (e) being handled well and step (d) mix is placed on and forms complex alloy powder in the container, adding quality is the binding agent Zinic stearas of complex alloy powder quality 0.5% again, add distilled water with its submergence, under electric mixer, stir 8h, the powder and the copper carbon fiber that stir are placed in the drying baker, 80 ℃ of oven dry 2h, the composite powder after then will drying is put into ball mill again and is dry mixed 6h;
Step (2), step (3) are identical with step (2), the step (3) of embodiment 1.
Embodiment 5
Prepare an Albatra metal-based self lubricated composite material, its chemical ingredients is Ni10%, Sm by mass percentage 2O 31%, MoS 21%, Ag1%, CaF 21%, Al 2O 32%, (chemical ingredients is Zn5% by mass percentage in the ZQSn663 tinbronze powder for W 3%, nickel plating graphite 3%, copper carbon fiber (diameter is 1 μ m) 2.5%, ZQSn663 tinbronze powder, Sn5%, Pb2%, copper 88%) 75.5%, its performance is as shown in table 1, and the preparation method is as follows:
(1) batch mixing: expect the mixing of powder with barrel at mixer, the mixer rotating speed is 400r/min, adds steel ball in the barrel and spring forms abrasive material, and making abrasive material and metallurgical volume ratio with composite powder is 7:1, is conducive to stirring and evenly mixes; Wherein metallurgy carries out according to the following steps with the composite powder batch mixing:
(a) take by weighing respectively Ni, Sm 2O 3, MoS 2, Ag, CaF 2, Al 2O 3, W, nickel plating graphite, copper carbon fiber and ZQSn663 tinbronze powder be stand-by, the amount of taking by weighing is Ni10%, Sm by mass percentage 2O 31%, MoS 21%, Ag1%, CaF 21%, Al 2O 32%, W 3%, nickel plating graphite 3%, copper carbon fiber 3.0%, ZQSn663 tinbronze powder 75.5%;
The nanometer Al that (b) will take by weighing 2O 3Powder and ZQSn663 bronze powder are put into mixing tank for 1:1 in mass ratio, add an amount of dehydrated alcohol as grinding medium, put the mixing of rolling in the ball mill after the sealing into, take out behind the rotating speed 400r/min wet mixing 7h of ball mill, it is stand-by to form the master alloy powder behind drying at room temperature, fragmentation, mistake 200 mesh sieves;
The W powder that (c) will take by weighing and ZQSn663 bronze powder form the master alloy powder by mass percentage for 1:1 is dry mixed 6h;
(d) get the nanometer Al of step (b) 2O 3The W powder master alloy powder of master alloy powder and step (c) adds Ni, the Sm that takes by weighing again 2O 3, MoS 2, Ag, CaF 2, nickel plating graphite and remaining ZQSn663 tinbronze powder, be dry mixed 6h, the compacting sample powder that evenly becomes to be mixed;
(e) get the copper carbon fiber that takes by weighing, being cut to the short carbon fiber that length is 1mm, is glycerine and the alcohol wiring solution-forming of 1:1 with volume ratio, with magnetic stirring apparatus the carbon fiber bubble is stirred 8h in solution, carbon fiber is spread out mutually, then clean with distilled water;
(f) powder that the copper carbon fiber of step (e) being handled well and step (d) mix is placed on and forms complex alloy powder in the container, adding quality is the binding agent Zinic stearas of complex alloy powder quality 0.5% again, add distilled water with its submergence, under electric mixer, stir 8h, the powder and the copper carbon fiber that stir are placed in the drying baker, 80 ℃ of oven dry 2h, the composite powder after then will drying is put into ball mill again and is dry mixed 5h;
Step (2), step (3) are identical with step (2), the step (3) of embodiment 1.
Embodiment 6
Prepare an Albatra metal-based self lubricated composite material, its chemical ingredients is Ni10%, Sm by mass percentage 2O 31%, MoS 21%, Ag1%, CaF 21%, Al 2O 32%, (chemical ingredients is Zn5% by mass percentage in the ZQSn663 tinbronze powder for W 3%, nickel plating graphite 3%, copper carbon fiber (diameter is 1 μ m) 3.0%, ZQSn663 tinbronze powder, Sn5%, Pb2%, copper 88%) 75.0%, its performance is as shown in table 1, and the preparation method is as follows:
(1) batch mixing: expect the mixing of powder with barrel at mixer, the mixer rotating speed is 400r/min, adds steel ball in the barrel and spring forms abrasive material, and making abrasive material and metallurgical volume ratio with composite powder is 7:1, is conducive to stirring and evenly mixes; Wherein metallurgy carries out according to the following steps with the composite powder batch mixing:
(a) take by weighing respectively Ni, Sm 2O 3, MoS 2, Ag, CaF 2, Al 2O 3, W, nickel plating graphite, copper carbon fiber and ZQSn663 tinbronze powder be stand-by, the amount of taking by weighing is Ni10%, Sm by mass percentage 2O 31%, MoS 21%, Ag1%, CaF 21%, Al 2O 32%, W 3%, nickel plating graphite 3%, copper carbon fiber 3.0%, ZQSn663 tinbronze powder 75.0%;
The nanometer Al that (b) will take by weighing 2O 3Powder and ZQSn663 bronze powder are put into mixing tank for 1:1 in mass ratio, add an amount of dehydrated alcohol as grinding medium, put the mixing of rolling in the ball mill after the sealing into, take out behind the rotating speed 400r/min wet mixing 7h of ball mill, it is stand-by to form the master alloy powder behind drying at room temperature, fragmentation, mistake 200 mesh sieves;
The W powder that (c) will take by weighing and ZQSn663 bronze powder form the master alloy powder by mass percentage for 1:1 is dry mixed 6h;
(d) get the nanometer Al of step (b) 2O 3The W powder master alloy powder of master alloy powder and step (c) adds Ni, the Sm that takes by weighing again 2O 3, MoS 2, Ag, CaF 2, nickel plating graphite and remaining ZQSn663 tinbronze powder, be dry mixed 6h, the compacting sample powder that evenly becomes to be mixed;
(e) get the copper carbon fiber that takes by weighing, being cut to the short carbon fiber that length is 1mm, is glycerine and the alcohol wiring solution-forming of 1:1 with volume ratio, with magnetic stirring apparatus the carbon fiber bubble is stirred 8h in solution, carbon fiber is spread out mutually, then clean with distilled water;
(f) powder that the copper carbon fiber of step (e) being handled well and step (d) mix is placed on and forms complex alloy powder in the container, adding quality is the binding agent Zinic stearas of complex alloy powder quality 0.5% again, add distilled water with its submergence, under electric mixer, stir 8h, the powder and the copper carbon fiber that stir are placed in the drying baker, 80 ℃ of oven dry 2h, the composite powder after then will drying is put into ball mill again and is dry mixed 5h;
Step (2), step (3) are identical with step (2), the step (3) of embodiment 1.
Table 1 is that other composition is identical, copper carbon fiber (C f) mechanical property and the frictional behaviour of new copper alloy-based composite self-lubricating material of the different preparation of content, as can be seen from Table 1, along with the increase of carbon fiber content, the porosity of the matrix material of preparation is increase trend, and the adding of carbon fiber has improved hardness, the crushing strength of material.When carbon fiber reached 2.5wt.%, the comprehensive mechanical property of matrix material was best, and hardness reaches 58HV, and the crushing strength value reaches 222MPa.Under 40N load, take rotating speed as 250r/min and 20 minutes frictional experiments of hardened steel (surface hardness HRC60) room temperature sliding friction show, in the abrasion loss of copper carbon fiber content matrix material in 0 ~ 2.5wt.% scope along with the increase that adds carbon fiber content is reduced to 4mg gradually by 12mg, when carbon fiber was 3wt.%, abrasion loss was in rising trend again.And presenting reduction trend thereupon, frictional coefficient has been reduced to 0.06 by 0.21.The new copper alloy composite self-lubricating material of present embodiment preparation, have different mechanical properties and frictional coefficient, the sample that wherein has high-wear resistance and low-friction coefficient 0.09, be applicable to the high-efficiency lubricating under the boundary lubrication condition, can be applied to the high precision friction parts under the low-speed heave-load condition.Fig. 2 is the stereoscan photograph that contains 2.5wt.% copper carbon fiber composite sample of embodiment 5 preparations, can observe the distribution situation in copper alloy matrix, solid lubrication phase and space from figure.
Table 1
Figure 785626DEST_PATH_IMAGE002
Embodiment 7
Prepare an Albatra metal-based self lubricated composite material, its chemical ingredients is Ni10%, Sm by mass percentage 2O 31%, MoS 21%, CaF 21%, Al 2O 32%, W3%, nickel plating graphite 3%, copper carbon fiber (diameter is 2 μ m) 2.5%, pore-forming material NH 4HCO 31.0%, ZQSn663 tinbronze powder (chemical ingredients is Zn7% by mass percentage in the ZQSn663 tinbronze powder, Sn7%, Pb4%, copper 82%) 75.5%, its performance is as shown in table 2, and the preparation method is as follows:
(1) batch mixing: expect the mixing of powder with barrel at mixer, the mixer rotating speed is 300r/min, adds steel ball in the barrel and spring forms abrasive material, and making abrasive material and metallurgical volume ratio with composite powder is 7:1, is conducive to stirring and evenly mixes; Wherein metallurgy carries out according to the following steps with the composite powder batch mixing:
(a) take by weighing respectively Ni, Sm 2O 3, MoS 2, CaF 2, Al 2O 3, W, nickel plating graphite, copper carbon fiber, pore-forming material NH 4HCO 3Stand-by with ZQSn663 tinbronze powder, the amount of taking by weighing is Ni10%, Sm by mass percentage 2O 31%, MoS 21%, CaF 21%, Al 2O 32%, W3%, nickel plating graphite 3%, copper carbon fiber 2.5%, pore-forming material NH 4HCO 31.0%, ZQSn663 tinbronze powder 75.5%;
The nanometer Al that (b) will take by weighing 2O 3Powder and ZQSn663 bronze powder are 1:1 wet mixing 8h in mass ratio, form the master alloy powder;
The W powder that (c) will take by weighing and ZQSn663 bronze powder form the master alloy powder in mass ratio for 1:1 is dry mixed 8h;
(d) get the nanometer Al of step (b) 2O 3The W powder master alloy powder of master alloy powder and step (c) adds Ni, the Sm that takes by weighing again 2O 3, MoS 2, CaF 2, nickel plating graphite and remaining ZQSn663 tinbronze powder, pour in the mixing machine that contains steel ball and spring, it is stand-by to be dry mixed 6h in the ball mill of packing into after the sealing;
(e) get the copper carbon fiber that takes by weighing, being cut to the short carbon fiber that length is about 2mm, is glycerine and the alcohol wiring solution-forming of 1:1 with volume ratio, with magnetic stirring apparatus the carbon fiber bubble is stirred 6h in solution, carbon fiber is spread out mutually, then clean with distilled water;
(f) powder that the copper carbon fiber of step (e) being handled well and step (d) mix is placed on and forms complex alloy powder in the container, adding quality is the binding agent Zinic stearas of complex alloy powder quality 1% again, add distilled water with its submergence, under electric mixer, stir 7h, the powder and the copper carbon fiber that stir are placed in the drying baker, 80 ℃ of oven dry 2h, the composite powder after then will drying is put into ball mill again and is dry mixed 5h;
The pore-forming material NH that (g) will take by weighing 4HCO 3Ball milling is dry mixed 5h in the powder of adding step (f) preparation, and then broken 200 mesh sieves of crossing become the powder metallurgy composite powder;
(2) sample compacting: a, weighing: according to the loose density of powder and the sintered density weighing of setting; B, dress mould: in the powder mould of packing into gently with weighing, with suitable power knock and the method that shakes make powder in die cavity, be evenly distributed as far as possible, smooth, with carrying out smoothly of assurance binder process; C, compacting: carry out Bidirectional pressure system at hydropress, predetermined pressing force is 563MPa, and slowly operation guarantees certain volume under pressure, and overflows pressurize 1min when reaching 563MPa for the more all even hole Airs that make the pressure transmission have enough time; D, the demoulding: after removing pressure, will eject in the sample from mould with special-purpose push rod, to be sintered;
(3) sintering of sample: the sample that suppresses is sintering under tube furnace hydrogen shield atmosphere, and the sintering hydrogen pressure is 0.7 ~ 0.8MPa, and sample is placed in the stainless steel sintering boat, uses Al 2O 3After sand covers sample, push the burner hearth middle part, close fire door, plugged is incubated 1h after being heated to 600 ℃ with the heat-up rate of 3 ℃/min, allow Zinic stearas decompose gradually and volatilize, avoid sintered compact surface cracking, foaming, buckling deformation, heat-up rate with 3 ℃/min is heated to 940 ℃ of insulation 4h again, then outage, under the condition of continuous protective atmosphere, sample is slided into the furnace roof position of the cold inner cover of water in advance, and water flowing cools to furnace temperature displays temperature (the actual sample regional temperature is lower than 200 ℃) below 350 ℃ with the furnace, close hydrogen after sample come out of the stove;
(4) the compound PTFE of hot dipping: sample is placed on 120 ℃ of oven dry 1h in the drying baker, in order to avoid have moisture in the hole of sample, affects the quality of PTFE hot dipping.Water-bath is heated to 60 ℃, sample is placed in the beaker that PTFE liquid is housed again, beaker is put into water-bath hot dipping 1.5h, the sample that hot dipping is good takes out, and is placed on 120 ℃ of oven dry in the drying baker, and preparation becomes new copper alloy-based composite self-lubricating material.
Embodiment 8
Prepare an Albatra metal-based self lubricated composite material, its chemical ingredients is Ni10%, Sm by mass percentage 2O 31%, MoS 21%, CaF 21%, Al 2O 32%, W3%, nickel plating graphite 3%, copper carbon fiber (diameter is 2 μ m) 2.5%, pore-forming material NH 4HCO 31.4%, ZQSn663 tinbronze powder (chemical ingredients is Zn7% by mass percentage in the ZQSn663 tinbronze powder, Sn7%, Pb4%, copper 82%) 75.1%, its performance is as shown in table 1, and its preparation method is as follows:
(1) batch mixing: expect the mixing of powder with barrel at mixer, the mixer rotating speed is 300r/min, adds steel ball in the barrel and spring forms abrasive material, and making abrasive material and metallurgical volume ratio with composite powder is 7:1, is conducive to stirring and evenly mixes; Wherein metallurgy carries out according to the following steps with the composite powder batch mixing:
(a) take by weighing respectively Ni, Sm 2O 3, MoS 2, CaF 2, Al 2O 3, W, nickel plating graphite, copper carbon fiber, pore-forming material NH 4HCO 3Stand-by with ZQSn663 tinbronze powder, the amount of taking by weighing is Ni10%, Sm by mass percentage 2O 31%, MoS 21%, CaF 21%, Al 2O 32%, W3%, nickel plating graphite 3%, copper carbon fiber 2.5%, pore-forming material NH 4HCO 31.4%, ZQSn663 tinbronze powder 75.1%;
The nanometer Al that (b) will take by weighing 2O 3Powder and ZQSn663 bronze powder are 1:1 wet mixing 8h in mass ratio, form the master alloy powder;
The W powder that (c) will take by weighing and ZQSn663 bronze powder form the master alloy powder in mass ratio for 1:1 is dry mixed 8h;
(d) get the nanometer Al of step (b) 2O 3The W powder master alloy powder of master alloy powder and step (c) adds Ni, the Sm that takes by weighing again 2O 3, MoS 2, CaF 2, nickel plating graphite and remaining ZQSn663 tinbronze powder, pour in the mixing machine that contains steel ball and spring, it is stand-by to be dry mixed 6h in the ball mill of packing into after the sealing;
(e) get the copper carbon fiber that takes by weighing, being cut to the short carbon fiber that length is 2mm, is glycerine and the alcohol wiring solution-forming of 1:1 with volume ratio, with magnetic stirring apparatus the carbon fiber bubble is stirred 6h in solution, carbon fiber is spread out mutually, then clean with distilled water;
(f) powder that the copper carbon fiber of step (e) being handled well and step (d) mix is placed on and forms complex alloy powder in the container, adding quality is the binding agent Zinic stearas of complex alloy powder quality 1% again, add distilled water with its submergence, under electric mixer, stir 7h, the powder and the copper carbon fiber that stir are placed in the drying baker 80 ℃ of oven dry 2h;
The pore-forming material NH that (g) will take by weighing 4HCO 3Add the middle ball milling of step (f) and be dry mixed 5h, then broken 200 mesh sieves of crossing become the powder metallurgy composite powder, and the composite powder after then will drying is put into ball mill again and is dry mixed 5h;
Step (2), (3), (4) are identical with step (2), (3), (4) of embodiment 7.
Embodiment 9
Prepare an Albatra metal-based self lubricated composite material, its chemical ingredients is Ni10%, Sm by mass percentage 2O 31%, MoS 21%, CaF 21%, Al 2O 32%, W3%, nickel plating graphite 3%, copper carbon fiber (diameter is 2 μ m) 2.5%, pore-forming material NH 4HCO 31.8%, ZQSn663 tinbronze powder (chemical ingredients is Zn7% by mass percentage in the ZQSn663 tinbronze powder, Sn7%, Pb4%, copper 82%) 74.7%, its performance is as shown in table 1, and its preparation method is as follows:
(1) batch mixing: expect the mixing of powder with barrel at mixer, the mixer rotating speed is 300r/min, adds steel ball in the barrel and spring forms abrasive material, and making abrasive material and metallurgical volume ratio with composite powder is 7:1, is conducive to stirring and evenly mixes; Wherein metallurgy carries out according to the following steps with the composite powder batch mixing:
(a) take by weighing respectively Ni, Sm 2O 3, MoS 2, CaF 2, Al 2O 3, W, nickel plating graphite, copper carbon fiber, pore-forming material NH 4HCO 3Stand-by with ZQSn663 tinbronze powder, the amount of taking by weighing is Ni10%, Sm by mass percentage 2O 31%, MoS 21%, CaF 21%, Al 2O 32%, W3%, nickel plating graphite 3%, copper carbon fiber 2.5%, pore-forming material NH 4HCO 31.8%, ZQSn663 tinbronze powder 74.7%;
The nanometer Al that (b) will take by weighing 2O 3Powder and ZQSn663 bronze powder are 1:1 wet mixing 8h in mass ratio, form the master alloy powder;
The W powder that (c) will take by weighing and ZQSn663 bronze powder form the master alloy powder in mass ratio for 1:1 is dry mixed 8h;
(d) get the nanometer Al of step (b) 2O 3The W powder master alloy powder of master alloy powder and step (c) adds Ni, the Sm that takes by weighing again 2O 3, MoS 2, CaF 2, nickel plating graphite and remaining ZQSn663 tinbronze powder, pour in the mixing machine that contains steel ball and spring, it is stand-by to be dry mixed 6h in the ball mill of packing into after the sealing;
(e) get the copper carbon fiber that takes by weighing, being cut to the short carbon fiber that length is 2mm, is glycerine and the alcohol wiring solution-forming of 1:1 with volume ratio, with magnetic stirring apparatus the carbon fiber bubble is stirred 6h in solution, carbon fiber is spread out mutually, then clean with distilled water;
(f) powder that the copper carbon fiber of step (e) being handled well and step (d) mix is placed on and forms complex alloy powder in the container, adding quality is the binding agent Zinic stearas of complex alloy powder quality 1% again, add distilled water with its submergence, under electric mixer, stir 7h, the powder and the copper carbon fiber that stir are placed in the drying baker, 80 ℃ of oven dry 2h, the composite powder after then will drying is put into ball mill again and is dry mixed 5h;
The pore-forming material NH that (g) will take by weighing 4HCO 3Ball milling is dry mixed 5h in the powder of adding step (f) preparation, and then broken 200 mesh sieves of crossing become the powder metallurgy composite powder;
Step (2), (3), (4) are identical with step (2), (3), (4) of embodiment 7.
Embodiment 10
Prepare an Albatra metal-based self lubricated composite material, its chemical ingredients is Ni10%, Sm by mass percentage 2O 31%, MoS 21%, CaF 21%, Al 2O 32%, W3%, nickel plating graphite 3%, copper carbon fiber (diameter is 2 μ m) 2.5%, pore-forming material NH 4HCO 32.2%, ZQSn663 tinbronze powder (chemical ingredients is Zn7% by mass percentage in the ZQSn663 tinbronze powder, Sn7%, Pb4%, copper 82%) 74.3%, its performance is as shown in table 2, and the preparation method is as follows:
(1) batch mixing: expect the mixing of powder with barrel at mixer, the mixer rotating speed is 300r/min, adds steel ball in the barrel and spring forms abrasive material, and making abrasive material and metallurgical volume ratio with composite powder is 7:1, is conducive to stirring and evenly mixes; Wherein metallurgy carries out according to the following steps with the composite powder batch mixing:
(a) take by weighing respectively Ni, Sm 2O 3, MoS 2, CaF 2, Al 2O 3, W, nickel plating graphite, copper carbon fiber, pore-forming material NH 4HCO 3Stand-by with ZQSn663 tinbronze powder, the amount of taking by weighing is Ni10%, Sm by mass percentage 2O 31%, MoS 21%, CaF 21%, Al 2O 32%, W3%, nickel plating graphite 3%, copper carbon fiber 2.5%, pore-forming material NH 4HCO 32.2%, ZQSn663 tinbronze powder 74.3%;
The nanometer Al that (b) will take by weighing 2O 3Powder and ZQSn663 bronze powder are 1:1 wet mixing 8h in mass ratio, form the master alloy powder;
The W powder that (c) will take by weighing and ZQSn663 bronze powder form the master alloy powder in mass ratio for 1:1 is dry mixed 8h;
(d) get the nanometer Al of step (b) 2O 3The W powder master alloy powder of master alloy powder and step (c) adds Ni, the Sm that takes by weighing again 2O 3, MoS 2, CaF 2, nickel plating graphite and remaining ZQSn663 tinbronze powder, pour in the mixing machine that contains steel ball and spring, it is stand-by to be dry mixed 6h in the ball mill of packing into after the sealing;
(e) get the copper carbon fiber that takes by weighing, being cut to the short carbon fiber that length is 2mm, is glycerine and the alcohol wiring solution-forming of 1:1 with volume ratio, with magnetic stirring apparatus the carbon fiber bubble is stirred 6h in solution, carbon fiber is spread out mutually, then clean with distilled water;
(f) powder that the copper carbon fiber of step (e) being handled well and step (d) mix is placed on and forms complex alloy powder in the container, adding quality is the binding agent Zinic stearas of complex alloy powder quality 1% again, add distilled water with its submergence, under electric mixer, stir 7h, the powder and the copper carbon fiber that stir are placed in the drying baker, 80 ℃ of oven dry 2h, the composite powder after then will drying is put into ball mill again and is dry mixed 5h;
The pore-forming material NH that (g) will take by weighing 4HCO 3Ball milling is dry mixed 5h in the powder of adding step (f) preparation, and then broken 200 mesh sieves of crossing become the powder metallurgy composite powder;
Step (2), (3), (4) are identical with step (2), (3), (4) of embodiment 7.
Embodiment 11
Prepare an Albatra metal-based self lubricated composite material, its chemical ingredients is Ni10%, Sm by mass percentage 2O 31%, MoS 21%, CaF 21%, Al 2O 32%, W3%, nickel plating graphite 3%, copper carbon fiber (diameter is 2 μ m) 2.5%, pore-forming material NH 4HCO 32.8%, ZQSn663 tinbronze powder (chemical ingredients is Zn7% by mass percentage in the ZQSn663 tinbronze powder, Sn7%, Pb4%, copper 82%) 73.7%, its performance is as shown in table 2, and the preparation method is as follows:
(1) batch mixing: expect the mixing of powder with barrel at mixer, the mixer rotating speed is 300r/min, adds steel ball in the barrel and spring forms abrasive material, and making abrasive material and metallurgical volume ratio with composite powder is 7:1, is conducive to stirring and evenly mixes; Wherein metallurgy carries out according to the following steps with the composite powder batch mixing:
(a) take by weighing respectively Ni, Sm 2O 3, MoS 2, CaF 2, Al 2O 3, W, nickel plating graphite, copper carbon fiber, pore-forming material NH 4HCO 3Stand-by with ZQSn663 tinbronze powder, the amount of taking by weighing is Ni10%, Sm by mass percentage 2O 31%, MoS 21%, CaF 21%, Al 2O 32%, W3%, nickel plating graphite 3%, copper carbon fiber 2.5%, pore-forming material NH 4HCO 32.8%, ZQSn663 tinbronze powder 73.7%;
The nanometer Al that (b) will take by weighing 2O 3Powder and ZQSn663 bronze powder are 1:1 wet mixing 5 ~ 8h in mass ratio, form the master alloy powder;
The W powder that (c) will take by weighing and ZQSn663 bronze powder form the master alloy powder in mass ratio for 1:1 is dry mixed 8h;
(d) get the nanometer Al of step (b) 2O 3The W powder master alloy powder of master alloy powder and step (c) adds Ni, the Sm that takes by weighing again 2O 3, MoS 2, CaF 2, nickel plating graphite and remaining ZQSn663 tinbronze powder, pour in the mixing machine that contains steel ball and spring, it is stand-by to be dry mixed 6h in the ball mill of packing into after the sealing;
(e) get the copper carbon fiber that takes by weighing, being cut to the short carbon fiber that length is 2mm, is glycerine and the alcohol wiring solution-forming of 1:1 with volume ratio, with magnetic stirring apparatus the carbon fiber bubble is stirred 6h in solution, carbon fiber is spread out mutually, then clean with distilled water;
(f) powder that the copper carbon fiber of step (e) being handled well and step (d) mix is placed on and forms complex alloy powder in the container, adding quality is the binding agent Zinic stearas of complex alloy powder quality 1% again, add distilled water with its submergence, under electric mixer, stir 7h, the powder and the copper carbon fiber that stir are placed in the drying baker, 80 ℃ of oven dry 2h, the composite powder after then will drying is put into ball mill again and is dry mixed 5h;
The pore-forming material NH that (g) will take by weighing 4HCO 3Ball milling is dry mixed 5h in the powder of adding step (f) preparation, and then broken 200 mesh sieves of crossing become the powder metallurgy composite powder;
Step (2), (3), (4) are identical with step (2), (3), (4) of embodiment 7.
Table 2 is different content NH 4HCO 3The mechanical property of pore-forming material sintered sample, the data from table can see that along with the continuous increase of pore-forming material body burden, the density of five groups of samples of sintering presents the trend of first increases and then decreases, void content presents the trend that reduces first rear increase, at NH 4HCO 3During for 1.8wt.%, the density of sample is maximum, and hardness and crushing strength maximum are respectively 35.5HV and 148MPa, and void content reaches 32%, has best over-all properties.
Table 2
Figure 702766DEST_PATH_IMAGE004
Fig. 3 is the 1.8wt.%NH that contains of embodiment 9 preparations 4HCO 3The scanning electron microscope shape appearance figure of composite sample, between blapharoplast and particle, exist as we can see from the figure a lot of holes, pore size does not wait, mean sizes is greatly about about 10 ~ 15 μ m, void distribution more even, what the A place referred among the figure is exactly the more typical hole that exists in the sample.
The sample that sintering is finished carries out hole consonance polytetrafluoroethylene PTFE to be processed, PTFE is the material of frictional coefficient minimum in the solid lubricant, form more concrete dynamic modulus through powder metallurgy pore-creating sintering, make the compound polymer PTFE of advancing material in the hole, formation has the new copper alloy-based composite self-lubricating material that the self-lubricating solid phase content reaches 30 ~ 40 vol.%, reaches the purpose that improves the composite material self-lubricating performance.
Embodiment 12
Prepare an Albatra metal-based self lubricated composite material, its chemical ingredients is Ni10%, Sm by mass percentage 2O 31%, MoS 21%, CaF 21%, Al 2O 32%, W3%, nickel plating graphite 3%, copper carbon fiber (diameter is 2 μ m) 2.5%, pore-forming material NH 4HCO 31.8%, ZQSn663 tinbronze powder (chemical ingredients is Zn7% by mass percentage in the ZQSn663 tinbronze powder, Sn7%, Pb4%, copper 82%) 74.7%, its preparation method is as follows:
Step (1), step (2), step (3) are identical with step (1), (2), (3) of embodiment 9;
(4) the compound PTFE of hot dipping: sample is placed on 120 ℃ of oven dry 1h in the drying baker, in order to avoid have moisture in the hole of sample, affects the quality of PTFE hot dipping.Water-bath is heated to 50 ℃, sample is placed in the beaker that PTFE liquid is housed again, beaker is put into water-bath hot dipping 1.5h, the sample that hot dipping is good takes out, and is placed on 120 ℃ of oven dry in the drying baker, and preparation becomes new copper alloy-based composite self-lubricating material.
Embodiment 13
Prepare an Albatra metal-based self lubricated composite material, its chemical ingredients is Ni10%, Sm by mass percentage 2O 31%, MoS 21%, CaF 21%, Al 2O 32%, W3%, nickel plating graphite 3%, copper carbon fiber (diameter is 2 μ m) 2.5%, pore-forming material NH 4HCO 31.8%, ZQSn663 tinbronze powder (chemical ingredients is Zn7% by mass percentage in the ZQSn663 tinbronze powder, Sn7%, Pb4%, copper 82%) 74.7%, its preparation method is as follows:
Step (1), step (2), step (3) are identical with step (1), (2), (3) of embodiment 9;
(4) the compound PTFE of hot dipping: sample is placed on 120 ℃ of oven dry 1h in the drying baker, in order to avoid have moisture in the hole of sample, affects the quality of PTFE hot dipping.Water-bath is heated to 70 ℃, sample is placed in the beaker that PTFE liquid is housed again, beaker is put into water-bath hot dipping 1.5h, the sample that hot dipping is good takes out, and is placed on 120 ℃ of oven dry in the drying baker, and preparation becomes new copper alloy-based composite self-lubricating material.
Fig. 4 contains 1.8wt.%NH 4HCO 3The scanning shape appearance figure of composite sample composite sample behind 50 ℃ (a), 60 ℃ (b) and 70 ℃ (c) lower hot dipping PTFE, from scintigram, more can be clear that, between particle and particle at the interface and the white PTFE that all distributing of hole place, enter into the content difference of the PTFE of sample under the different hot dipping temperature, when the hot dipping temperature was 60 ℃, the PTFE in the sample was maximum.
Fig. 5 is the 1.8wt.%NH that contains of embodiment 9 preparations 4HCO 3The line sweep figure of composite sample sample behind 60 ℃ of lower hot dipping PTFE, as can be seen from the figure, the hole place of every line sweep process, the peak that F and C have nearly all occurred, the peak of their correspondences of place that hole is larger is just higher, hot dippings PTFE that entered has been described in the hole in the sample, and this raising to the self-lubricating property of sample has Main Function.
Fig. 6 is the 1.8wt.%NH that contains of embodiment 9 preparations 4HCO 3The X-ray diffraction analysis of the sample of composite sample behind 60 ℃ of lower hot dipping PTFE, as we can see from the figure, the matrix of sample mainly is to be comprised of Cu and (Cu, Zn), (Cu, Sn) sosoloid, except other mutually, detected (C 2F 4) nDiffraction peak, this is tetrafluoroethylene (PTFE), proves that PTFE has entered into the sample of porous, has formed the self-lubricating material of Multiphase Complex Structure structure.
Choose 60 ℃ of samples behind the lower hot dipping PTFE and do not have hot dipping PTFE sample to carry out friction-wear test.Frictional wear experiment condition load 40N, rotating speed is 250r/min, sample and hardened steel (surface hardness HRC60) room temperature sliding friction 20 minutes (sliding distance is 942mm).Experiment shows that not having the abrasion loss of the sample of hot dipping PTFE is 21mg, and the abrasion loss of the sample behind the hot dipping PTFE only is 6mg.Fig. 7 is at 60 ℃ of lower hot dipping PTFE(a) and do not have hot dipping PTFE(b) frictional coefficient of composite sample changes comparison diagram in time, sample frictional coefficient behind the hot dipping PTFE will be well below the sample that does not have hot dipping, the sample stable friction factor stage of hot dipping PTFE is 0.08 only, is 0.26 and there is not the sample frictional coefficient of hot dipping.Therefore, in friction process, the PTFE in the space can squeezedly out cover on the surface of sample, has so just formed the more stable continuous lubricant film of one deck between sample surfaces and friction pair part.And the PTFE that is extruded can with same squeezed graphite, CaF out 2, MoS 2Form together one deck the compound lubricating film etc. lubricated phase, Effective Raise the wear resisting property of sample.
Fig. 8 be behind 60 ℃ of hot dipping PTFE sample and do not have the wearing and tearing of hot dipping PTFE sample after the scanning shape appearance figure.Can see many abrasive dusts and some pits from Fig. 8 (b), and fracture phenomena has also occured in lubricant film.Can see that from Fig. 8 (a) friction surface is covered with the material of large stretch of white, mainly be the solid lubricant film that PTFE forms in friction process, can avoid two friction surfaces directly to contact, and the material friction coefficient is reduced, and wearing and tearing steadily.The hole of PTFE is compound to have effectively reduced abrasion loss and the frictional coefficient of preparation material, proves that this new copper alloy-based composite self-lubricating material has better self-lubricating property, is adapted to lowly at a high speed carry, temperature is lower than under 350 ℃ of working conditions the friction axle sleeve and uses.
Embodiment 14
Prepare an Albatra metal-based self lubricated composite material, its chemical ingredients is Ni9%, Sm by mass percentage 2O 30.5%, MoS 20.5%, Ag1%, CaF 22%, Al 2O 31%, W 1%, nickel plating graphite 1%, copper carbon fiber (diameter is 1.5 μ m) 2.5%, ZQSn663 tinbronze powder (chemical ingredients is Zn6%, Sn6%, Pb3%, copper 85% by mass percentage in the ZQSn663 tinbronze powder) 81.5%, its preparation method is as follows:
(1) batch mixing: expect the mixing of powder with barrel at mixer, the mixer rotating speed is 350r/min, adds steel ball in the barrel and spring forms abrasive material, and making abrasive material and metallurgical volume ratio with composite powder is 7:1, is conducive to stirring and evenly mixes; Wherein metallurgy carries out according to the following steps with the composite powder batch mixing:
(a) take by weighing respectively Ni, Sm 2O 3, MoS 2, Ag, CaF 2, Al 2O 3, W, nickel plating graphite, copper carbon fiber and ZQSn663 tinbronze powder be stand-by, the amount of taking by weighing is Ni9%, Sm by mass percentage 2O 30.5%, MoS 20.5%, Ag1%, CaF 22%, Al 2O 31%, W 1%, nickel plating graphite 1%, copper carbon fiber 2.5%, ZQSn663 tinbronze powder 81.5%;
The nanometer Al that (b) will take by weighing 2O 3Powder and ZQSn663 bronze powder are put into mixing tank for 1:1 in mass ratio, add an amount of dehydrated alcohol as grinding medium, put the mixing of rolling in the ball mill after the sealing into, take out behind the rotating speed 350r/min wet mixing 5h of ball mill, it is stand-by to form the master alloy powder behind drying at room temperature, fragmentation, mistake 200 mesh sieves;
The W powder that (c) will take by weighing and ZQSn663 bronze powder form the master alloy powder in mass ratio for 1:1 is dry mixed 5h;
(d) get the nanometer Al of step (b) 2O 3The W powder master alloy powder of master alloy powder and step (c) adds Ni, the Sm that takes by weighing again 2O 3, MoS 2, Ag, CaF 2, nickel plating graphite and remaining ZQSn663 tinbronze powder, be dry mixed 7h, the compacting sample powder that evenly becomes to be mixed;
(e) get the copper carbon fiber that takes by weighing, being cut to the short carbon fiber that length is 2mm, is glycerine and the alcohol wiring solution-forming of 1:1 with volume ratio, with magnetic stirring apparatus the carbon fiber bubble is stirred 6h in solution, carbon fiber is spread out mutually, then clean with distilled water;
(f) powder that the copper carbon fiber of step (e) being handled well and step (d) mix is placed on and forms complex alloy powder in the container, adding quality is the binding agent Zinic stearas of complex alloy powder quality 0.5% again, add distilled water with its submergence, under electric mixer, stir 8h, the powder and the copper carbon fiber that stir are placed in the drying baker, 80 ℃ of oven dry 2h, the composite powder after then will drying is put into ball mill again and is dry mixed 5h;
(2) sample compacting: a, weighing: according to the loose density of powder and the sintered density weighing of setting; B, dress mould: in the powder mould of packing into gently with weighing, with suitable power knock and the method that shakes make powder in die cavity, be evenly distributed as far as possible, smooth, with carrying out smoothly of assurance binder process; C, compacting: carry out Bidirectional pressure system at hydropress, predetermined pressing force is 563MPa, and slowly operation guarantees certain volume under pressure, and overflows pressurize 1min when reaching 563MPa for the more all even hole Airs that make the pressure transmission have enough time; D, the demoulding: after removing pressure, will eject in the sample from mould with special-purpose push rod, to be sintered;
(3) sintering of sample: the sample that suppresses is sintering under tube furnace hydrogen shield atmosphere, and the sintering hydrogen pressure is 0.7 ~ 0.8MPa, and sample is placed in the stainless steel sintering boat, uses Al 2O 3After sand covers sample; push the burner hearth middle part; close fire door; plugged is incubated 1h after being heated to 600 ℃ with the heat-up rate of 3 ℃/min; allow Zinic stearas decompose gradually and volatilize; avoid sintered compact surface cracking, foaming, buckling deformation; heat-up rate with 3 ℃/min is heated to 940 ℃ of insulation 4h again; then outage; under the condition of continuous protective atmosphere; sample is slided into the furnace roof position of the cold inner cover of water in advance, and water flowing cools to furnace temperature displays temperature (the actual sample regional temperature is lower than 200 ℃) below 350 ℃ with the furnace, close hydrogen after sample come out of the stove.
Embodiment 15
Prepare an Albatra metal-based self lubricated composite material, its chemical ingredients is Ni9.5%, Sm by mass percentage 2O 30.7%, MoS 20.8%, CaF 21.5%, Al 2O 31.5%, nickel plating graphite 2%, copper carbon fiber (diameter is 1 μ m) 2.5%, pore-forming material NH 4HCO 31.8%, ZQSn663 tinbronze powder (chemical ingredients is Zn6% by mass percentage in the ZQSn663 tinbronze powder, Sn6%, Pb3%, copper 85%) 79.7%, its preparation method is as follows:
(1) batch mixing: expect the mixing of powder with barrel at mixer, the mixer rotating speed is 300r/min, adds steel ball in the barrel and spring forms abrasive material, and making abrasive material and metallurgical volume ratio with composite powder is 7:1, is conducive to stirring and evenly mixes; Wherein metallurgy carries out according to the following steps with the composite powder batch mixing:
(a) take by weighing respectively Ni, Sm 2O 3, MoS 2, CaF 2, Al 2O 3, nickel plating graphite, copper carbon fiber, pore-forming material NH 4HCO 3Stand-by with ZQSn663 tinbronze powder, the amount of taking by weighing is Ni9.5%, Sm by mass percentage 2O 30.7%, MoS 20.8%, CaF 21.5%, Al 2O 31.5%, nickel plating graphite 2%, copper carbon fiber 2.5%, pore-forming material NH 4HCO 31.8%, ZQSn663 tinbronze powder 79.7%;
The nanometer Al that (b) will take by weighing 2O 3Powder and ZQSn663 bronze powder are 1:1 wet mixing 5h in mass ratio, form the master alloy powder;
(c) get the nanometer Al of step (b) 2O 3The master alloy powder adds Ni, the Sm that takes by weighing again 2O 3, MoS 2, CaF 2, nickel plating graphite and remaining ZQSn663 tinbronze powder, pour in the mixing machine that contains steel ball and spring, it is stand-by to be dry mixed 6h in the ball mill of packing into after the sealing;
(d) get the copper carbon fiber that takes by weighing, being cut to the short carbon fiber that length is 1mm, is glycerine and the alcohol wiring solution-forming of 1:1 with volume ratio, with magnetic stirring apparatus the carbon fiber bubble is stirred 6h in solution, carbon fiber is spread out mutually, then clean with distilled water;
(e) powder that the copper carbon fiber of step (d) being handled well and step (c) mix is placed on and forms complex alloy powder in the container, adding quality is the binding agent Zinic stearas of complex alloy powder quality 0.8% again, add distilled water with its submergence, under electric mixer, stir 7h, the powder and the copper carbon fiber that stir are placed in the drying baker, 80 ℃ of oven dry 2h, the composite powder after then will drying is put into ball mill again and is dry mixed 5h;
The pore-forming material NH that (f) will take by weighing 4HCO 3Ball milling is dry mixed 6h in the powder of adding step (e) preparation, and then broken 200 mesh sieves of crossing become the powder metallurgy composite powder;
(2) sample compacting: a, weighing: according to the loose density of powder and the sintered density weighing of setting; B, dress mould: in the powder mould of packing into gently with weighing, with suitable power knock and the method that shakes make powder in die cavity, be evenly distributed as far as possible, smooth, with carrying out smoothly of assurance binder process; C, compacting: carry out Bidirectional pressure system at hydropress, predetermined pressing force is 563MPa, and slowly operation guarantees certain volume under pressure, and overflows pressurize 1min when reaching 563MPa for the more all even hole Airs that make the pressure transmission have enough time; D, the demoulding: after removing pressure, will eject in the sample from mould with special-purpose push rod, to be sintered;
(3) sintering of sample: the sample that suppresses is sintering under tube furnace hydrogen shield atmosphere, and the sintering hydrogen pressure is 0.7 ~ 0.8MPa, and sample is placed in the stainless steel sintering boat, uses Al 2O 3After sand covers sample, push the burner hearth middle part, close fire door, plugged is incubated 1h after being heated to 600 ℃ with the heat-up rate of 3 ℃/min, allow Zinic stearas decompose gradually and volatilize, avoid sintered compact surface cracking, foaming, buckling deformation, heat-up rate with 3 ℃/min is heated to 940 ℃ of insulation 4h again, then outage, under the condition of continuous protective atmosphere, sample is slided into the furnace roof position of the cold inner cover of water in advance, and water flowing cools to furnace temperature displays temperature (the actual sample regional temperature is lower than 200 ℃) below 350 ℃ with the furnace, close hydrogen after sample come out of the stove;
The sample that sintering is finished carries out hole consonance polytetrafluoroethylene PTFE to be processed, PTFE is the material of frictional coefficient minimum in the solid lubricant, form more concrete dynamic modulus through powder metallurgy pore-creating sintering, make the compound polymer PTFE of advancing material in the hole, formation has the new copper alloy-based composite self-lubricating material that the self-lubricating solid phase content reaches 30 ~ 40 vol.%, reaches the purpose that improves the composite material self-lubricating performance.
(4) the compound PTFE of hot dipping: with pore-forming material NH 4HCO 3Content is that the sample of 1.8wt.% is placed on 120 ℃ of oven dry 1h in the drying baker, in order to avoid have moisture in the hole of sample, affects the quality of PTFE hot dipping.Water-bath is heated to 60 ℃, ready sample is placed in the beaker that PTFE liquid is housed again, beaker is put into water-bath hot dipping 1.5h, the sample that hot dipping is good takes out, be placed on 120 ℃ of oven dry in the drying baker, preparation becomes new copper alloy-based composite self-lubricating material.

Claims (4)

1. an Albatra metal-based self lubricated composite material is characterized in that its chemical ingredients is by mass percentage: Ni 9 ~ 10%, Sm 2O 30.5 ~ 1%, MoS 20.5 ~ 1%, Ag 0 ~ 1%, CaF 20 ~ 2%, Al 2O 31 ~ 2%, W 0 ~ 3%, nickel plating graphite 1 ~ 3%, copper carbon fiber 1.1 ~ 3.0%, pore-forming material NH 4HCO 30 ~ 2.8%, ZQSn663 tinbronze powder 73.7 ~ 81.5%, and its density is 4.71 ~ 6.54g/cm 3, hardness is 30 ~ 58HV, crushing strength 99 ~ 222MPa, frictional coefficient are 0.15 ~ 0.06.
2. an Albatra metal-based self lubricated composite material according to claim 1 is characterized in that the chemical ingredients of described ZQSn663 tinbronze powder is Zn5 ~ 7% by mass percentage, Sn5 ~ 7%, and Pb2 ~ 4%, surplus is copper.
3. an Albatra metal-based self lubricated composite material according to claim 1 is characterized in that described copper carbon fiber diameter is 1 ~ 2 μ m, and length is 1 ~ 2mm.
4. the preparation method of an Albatra metal-based self lubricated composite material is characterized in that may further comprise the steps:
(1) batch mixing: expect the mixing of powder with barrel at mixer, the mixer rotating speed is 300 ~ 400r/min, adds steel ball in the barrel and spring forms abrasive material, and making abrasive material and metallurgical volume ratio with composite powder is 7:1; Wherein metallurgy carries out according to the following steps with the composite powder batch mixing:
(a) take by weighing respectively Ni, Sm 2O 3, MoS 2, Ag, CaF 2, Al 2O 3, W, nickel plating graphite, copper carbon fiber, pore-forming material NH 4HCO 3Stand-by with ZQSn663 tinbronze powder, the amount of taking by weighing is Ni 9 ~ 10%, Sm by mass percentage 2O 30.5 ~ 1%, MoS 20.5 ~ 1%, Ag 0 ~ 1%, CaF 20 ~ 2%, Al 2O 31 ~ 2%, W 0 ~ 3%, nickel plating graphite 1 ~ 3%, copper carbon fiber 1.1 ~ 3.0%, pore-forming material NH 4HCO 30 ~ 2.8%, ZQSn663 tinbronze powder 73.7 ~ 81.5%;
The nanometer Al that (b) will take by weighing 2O 3Powder and ZQSn663 tinbronze powder be 1:1 wet mixing 5 ~ 8h in mass ratio, forms the master alloy powder;
The W powder that (c) will take by weighing and ZQSn663 tinbronze powder form the master alloy powder in mass ratio for 1:1 is dry mixed 5 ~ 8h;
(d) get the nanometer Al of step (b) 2O 3The W powder master alloy powder of master alloy powder and step (c) adds Ni, the Sm that takes by weighing again 2O 3, MoS 2, Ag, CaF 2, nickel plating graphite and remaining ZQSn663 tinbronze powder be dry mixed 6 ~ 8h, the compacting sample powder that evenly becomes to be mixed;
(e) get the copper carbon fiber that takes by weighing, being cut to the short carbon fiber that length is 1 ~ 2mm, is glycerine and the alcohol wiring solution-forming of 1:1 with volume ratio, with magnetic stirring apparatus the carbon fiber bubble is stirred 5 ~ 8h in solution, carbon fiber is spread out mutually, then clean with distilled water;
(f) powder that the copper carbon fiber of step (e) being handled well and step (d) mix is placed on and forms complex alloy powder in the container, adding quality is the binding agent Zinic stearas of complex alloy powder quality 0.5 ~ 1% again, add distilled water with its submergence, under electric mixer, stir 8h, the powder and the copper carbon fiber that stir are placed in the baking oven, 80 ℃ of oven dry, the composite powder after then will drying is put into ball mill again and is dry mixed 4 ~ 8h;
The pore-forming material NH that (g) will take by weighing 4HCO 3Be dry mixed 5 ~ 6h in the powder of adding step (f) preparation, become the metallurgical composite powder of using;
(2) sample compacting: according to the loose density of powder and the sintered density weighing of setting, sample carry out Bidirectional pressure system at hydropress, guarantee in the pressing process to pressurize evenly, slowly and the release of pressure process, then reach pressurize 1min behind the predetermined pressing pressure 563MPa, so that gas can be discharged smoothly, guarantee that simultaneously powder fully tamps in die cavity;
(3) sintering of sample: the sample that suppresses is sintering under tube furnace hydrogen shield atmosphere, the sintering hydrogen pressure is 0.7 ~ 0.8MPa, be incubated 1h after being heated to 600 ℃ with the heat-up rate of 3 ℃/min, then be heated to 940 ℃ with the heat-up rate of 3 ℃/min and carry out heat preservation sintering 4h, then outage, under the condition of continuous protective atmosphere, be lower than 200 ℃ with the stove water cooling to the sample area temperature after sample come out of the stove;
(4) sample after sintering is finished carries out the compound PTFE of hot dipping: water-bath is heated to 50 ℃ ~ 70 ℃, again the sample that sinters is placed in the beaker that PTFE liquid is housed, beaker is put into water-bath hot dipping 1.5h, sample that hot dipping is good takes out, and is placed on that 120 ℃ of oven dry are prepared into matrix material in the drying baker; If the pore-forming material addition is 0, then need not carry out this step.
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