CN105132736A - Dispersed copper composite material and preparation method thereof - Google Patents

Dispersed copper composite material and preparation method thereof Download PDF

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CN105132736A
CN105132736A CN201510551047.1A CN201510551047A CN105132736A CN 105132736 A CN105132736 A CN 105132736A CN 201510551047 A CN201510551047 A CN 201510551047A CN 105132736 A CN105132736 A CN 105132736A
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powder
preparation
matrix material
powdered alloy
extrusion
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CN105132736B (en
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田保红
张毅
李武会
龙永强
李红霞
任凤章
贾淑果
刘勇
宋克兴
李全安
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Henan University of Science and Technology
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Henan University of Science and Technology
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Abstract

The invention discloses a dispersed copper composite material and a preparation method thereof, belonging to the technical field of dispersed copper processing. The dispersed copper composite material is composed of the following components in percentage by mass: 0.24-3.74% of Al2O3, 0.03-1.27% of Y2O3 and the balance of Cu and unavoidable impurities. The dispersed copper composite material is prepared from Cu2O powder and Cu-Al-Y alloy powder through the steps of mixing, pressing, sintering and internal oxidation, extruding and forging; the composite material has the high strength of 500Pa or above and the high conductivity of 80% IACS or above and overcomes the defect that the high strength and high conductivity of other composite materials cannot simultaneously exist; and meanwhile the composite material is favorable in softening resistance, high in high-temperature strength and good in plasticity, and the softening temperature is 800 DEG C or higher.

Description

Dispersion copper matrix material and preparation method thereof
Technical field
The present invention relates to a kind of dispersion copper matrix material, also relate to the preparation method of dispersion copper matrix material simultaneously, belong to dispersion copper processing technique field.
Background technology
As the Al of disperse phase 2o 3particle is to Cu-Al 2o 3the contribution of composite material strength is mainly manifested in the following aspects (1) Al 2o 3particle pinning dislocation, under certain condition as dislocation source, increases dislocation desity; (2) Al 2o 3the existence of particle hinders the motion of dislocation, subgrain boundary, thus hinders formation and the grain growth of recrystallize nucleus; (3) Al 2o 3the existence of particle can suppress the carrying out of Static and dynamic recrystallize.Therefore, Cu-Al 2o 3matrix material has the advantages such as high thermal conductivity, high conductivity and excellent hot strength, high-temperature creep resistance, wear resisting property be good, has huge application potential, caused people to study interest widely in fields such as electromechanics, electronics, aerospace and nuclear power.
The preparation of ODS copper-base alloys, key be how to obtain ultra-fine alumina particle and make its equably Dispersed precipitate on Copper substrate, guarantee high conductance while improve its mechanical behavior under high temperature.Conventional preparation method mainly contains: the powder metallurgic method of prior powder metallurgy method and improvement, comprises mechanical alloying method, coprecipitation method, sol-gel method, local reduction way etc.Emerge many dispersion-strengthened Cu new preparation technologies in recent years, as reactive spray-deposition, vacuum mixing casting, XD method and internal oxidation etc., its main purpose is the production cost keeping the basis of traditional dispersion-strengthened Cu product properties reducing dispersion-strengthened Cu, to promote applying of dispersion-strengthened Cu.Wherein Cu-Al powdered alloy internal oxidation is the Cu-Al that current commercialization processability is excellent 2o 3the optimal path of matrix material.As the Cu-0.7Al that SCM Corporation of the U.S. prepares with internal oxidation 2o 3matrix material, tensile strength reaches 585Ma, and unit elongation is 11%, specific conductivity 85%IACS, and has excellent anti-softening temperature.Domestic also have a lot of units research internal oxidation to prepare Cu-Al 2o 3matrix material, the wherein Cu-0.62Al for preparing of University Of Tianjin 2o 3matrix material, tensile strength reaches 608Ma, specific conductivity 80%IACS.
Traditional internal oxidation prepares Cu-Al 2o 3the technique of alloy is: first carry out preparing burden according to Al content requirement and in induction furnace melting Cu-Al alloy, then adopt water atomization or N 2atomization Cu-Al alloy melt becomes Cu-Al powdered alloy.By dried Cu-Al powdered alloy and Cu 2o powder mixes, and then mixed powder is put into vacuum oven and be heated to 800 ~ 1000 DEG C, held for some time carries out internal oxidition.Controlling oxygen partial pressure makes the Al in Cu-Al alloy oxidized, and Cu is not oxidized.Internal oxidition terminates just to obtain Cu-Al 2o 3the Cu of powder and Cu powder and remnants 2the mixed powder of O.Pass into H again 2remove residual oxygen, just obtain Cu-Al 2o 3powder and Cu powder.Carry out jacket again, vacuumize, isostatic pressed base, then hot extrusion, obtain extrusion blank, then cold-drawn obtains required section bar.
But traditional internal oxidation prepares Cu-Al 2o 3also there is many problems in matrix material: (1) operation is many, and the cycle is long, and production cost is high, can not manufacture large size and complex-shaped part; (2) influence factor is too many, and production process is wayward, and quality of materials is unstable; (3) be difficult to realize automatization, mass-producing, continuous seepage, so be difficult to apply.For car body welding producing line spot-wedling electrode, the Cr-Zr-Cu bar cost that current spot-wedling electrode is conventional is about 60,000 yuan/ton, adopts Cu-Al prepared by traditional internal oxidation process 2o 3the cost of matrix material is about 150,000 yuan/ton, although Cu-Al 2o 3the work-ing life of composite electrode is more than 3 times of traditional C r-Zr-Cu electrode, but cost is also up to 2.5 times, adds the custom using producer, is difficult to apply.This is also current Cu-Al 2o 3the subject matter that matrix material faces in applying.Therefore, design new dispersion copper contact material, develop new technology of preparing with Simplified flowsheet, reduce costs, raise the efficiency, expand the scale of production, become a very important task.
The patent of invention of publication number CN101338389A discloses the preparation method of a kind of integral dispersion copper rare-earth copper alloy material and dispersion copper, rare-earth copper alloy material mainly comprises Cu, Al and rare earth addition RE, each component content is: Al0.1 ~ 1wt%, RE0.05 ~ 0.5wt%, surplus is Cu, and its middle-weight rare earths RE refers to Y or Ce or mixed rare-earth elements (Ce+Y).The preparation method of dispersion copper comprises: the 1) melting of alloy: heat up after being melted by Cu-CATH-1 (purity 99.95%) refining, then adds Al insulation melting, and under Ar gas shielded, add Y, casting after fully stirring, cooling is come out of the stove; 2) hot-work of alloy: carry out hot extrusion or hot rolling in 4 ~ 8 hours in temperature 850 ~ 950 DEG C insulation; 3) solid solution of alloy: the temperature of solution treatment is 900 ~ 950 DEG C, and soaking time 2 ~ 4 hours, carries out shrend after solution treatment; 4) cold deformation: point passes of drawing process.Dispersion copper prepared by the method has the feature such as high strength & high electric-conduction, high resistance softening temperature, but its intensity and electric conductivity still have much room for improvement.
Summary of the invention
The object of this invention is to provide a kind of dispersion copper matrix material with high strength, high conductivity and good mechanical behavior under high temperature.
Meanwhile, the present invention also provides a kind of preparation method of dispersion copper matrix material.
In order to realize above object, the technical solution adopted in the present invention is:
Dispersion copper matrix material, is made up of the component of following mass percent: Al 2o 30.24 ~ 3.74%, Y 2o 30.03 ~ 1.27%, surplus is Cu and inevitable impurity.
For the preparation of the powder of dispersion copper matrix material, be made up of the component of following mass percent: 1.22 ~ 21.79%Cu 2o powder, surplus is Cu-Al-Y powdered alloy; Preferably, Cu 2o powder 1.58 ~ 18.96%, surplus is Cu-Al-Y powdered alloy.The mass percent that Al and Y accounts for 0.25 ~ 2.0%, Al and Y of Cu-Al-Y powdered alloy quality is altogether (25% ~ 90%): (10% ~ 75%).Cu 2the addition of O is generally 120% of requisite oxygen, and unnecessary oxygen can, by assembling effusion, only have minute quantity can exist with the form of CuAlO compound at high temperature, and very little on electric conductivity impact, intensity rises on the contrary.
Described Cu 2the granularity of O powder is-325 order+400 orders (namely by 325 orders but not by 400 orders), purity>=99.0%.
The granularity of described Cu-Al-Y powdered alloy is-270 order+400 orders (namely by 270 orders but not by 400 orders).It is obtained through melting, powder by atomization technique by raw material Cu, Al, Y.Raw material Cu can select standard cathode copper Cu-CATH-2, Cu content >=99.95wt%; Al can select remelting aluminium ingot Al99.70, Al content >=99.70wt%; Y can select rare earth metal yttrium Y-1, Y content >99.5%.
In the present invention, Rare Earth Y mainly contains the effect of two aspects, and one is that micro-Y purifies melt and crystal grain thinning in alloy melting, generates high-melting-point Y by metallurgical reaction 2o 3promote forming core crystal grain thinning and second-phase dispersion strengthening, two is by additional oxidizer, internal oxidition reaction original position is occurred Y unoxidized in alloy to be formed and the compact nanometer Y of matrix 2o 3, the Al produced with internal oxidition 2o 3acting in conjunction, to produce the dispersion-strengthened effect mixing type of metal oxide compound.Further, Al, Y of adding can produce more stable oxide structure by metallurgical reaction in atomization process, as produced α-Al 2o 3, be different from γ-Al internal oxidition only occurring and produces 2o 3.
Research shows, in the preparation process of Cu-Al-Y powdered alloy, no matter be water atomization or general industry nitrogen atomization, always generate by metallurgical reaction the nonmetallic compound that small part is insoluble to acid in prepared Cu-Al-Y powdered alloy, XRD analysis is indicated as α-Al 2o 3and Y 2o 3.Therefore, the oxide dispersion intensifying copper prepared by atomization and internal oxidition, the source of its oxide compound is different, and structure is different, and corresponding strengthening mechanism is not identical yet.
With Cu 2o powder carries out internal oxidition after doing the Cu-Al-Y mixed powder for alloy compacting of oxygen source, at certain temperature and atmosphere, and Cu 2o resolves into Cu and [O]; [O] adsorbs and dissolves in Cu-Al-Y alloying pellet surface; [O] spreads at matrix Cu and becomes Al with Al preferential oxidation in matrix 2o 3, complete internal oxidition, obtain the Cu-(Al of dispersion-strengthened 2o 3+ Y 2o 3) matrix material.In this process, because [O] spread coefficient in copper is far longer than the spread coefficient of Al and Y in copper, therefore can think in-situ preparation Al 2o 3+ Y 2o 3.
Carry out oxygenant Cu 2when O content is selected, consider following factor: containing impurity elements such as phosphorus in (1) Cu-Al-Y powdered alloy, order arrangement by size, if the elements such as P, Al, As, Fe, Ni, Mg, Sn, Si and Zn and copper form the specific conductivity that sosoloid greatly will reduce copper alloy, therefore to as much as possible impurity element be oxidized; (2) as the Cu of oxygen source 2cu-Al-Y powdered alloy surface can not be adsorbed in after O pyrolytic decomposition completely and complete diffusion; (3) actual mechanical process can not so accurately control various parameter as Theoretical Calculation.
The preparation method of dispersion copper matrix material is: by Cu 2o powder and Cu-Al-Y powdered alloy fully mix rear press forming and obtain billet, and billet is extrusion molding after the process of sintering internal oxidition, and forging, to obtain final product.
(1) compacting of powdered alloy
During tradition compacting, under the pressure of stamping, mixed powder shows and character like liquid phase to a certain extent, namely to all directions flowing, thus produces wall pressure to pressing mold wall.But due to intergranular friction, wedging and other factors, make pressure in the transmission of sidewall direction than much smaller in the transmission of pressing direction.Produce frictional force between outer coating powder and die wall, its size increases with the increase of pressing pressure.Friction makes compressing occur significant Pressure Drop in the height direction.The ununiformity of pressure distribution will cause the density of pressed compact each several part also uneven.Adopt isostatic cool pressing can improve density distribution uniformity and the density of blank.
If keep certain hour under a certain specific pressure, often extraordinary effect can be obtained.The reason of pressurize is: (1) makes pressure transmission abundant, is conducive to the density distribution of each several part in pressed compact; (2) air in body of powder hole is made to have time enough to overflow; (3) to the mechanical engagement between powder and deformation time, the carrying out of strain relaxation is conducive to.
Pressing speed in pressing process not only has influence on Frotteurism between powder particle and work hardening capacity, and has influence on air from the interpore effusion situation of powder particle.If pressing speed is too fast, air effusion just difficulty, makes the defect in pressed compact increase.Therefore, the pressing process such as cold should be carried out with slow pressurized state.
To sum up, the present invention adopts room temperature isostatic cool pressing to suppress, and pressure is 270 ~ 380MPa, and pressing speed is 40 ~ 60MPa/min (is generally carried in 2 ~ 3min and completes), and the dwell time is 2 ~ 10min.
(2) sintering-internal oxidition of powder
Because the diffusion of Al, [O] and chemical reaction velocity exponentially increase with the raising of temperature, therefore, improve internal oxidition temperature and can greatly shorten internal oxidition required time, but during more than 1000 DEG C internal oxidition, hardness value obviously reduces, and this is relevant with growing up of particle.Therefore internal oxidition temperature is unsuitable too high, generally should more than 1000 DEG C.Internal oxidition mainly occurs in shorter for some time at initial stage, prolongation in time, and Internal oxidation rate sharply declines, and the actual internal oxidition time is unsuitable long.
To sum up, in the present invention, the temperature of sintering-internal oxidition is 950 ~ 1000 DEG C, and soaking time is 2 ~ 10h.
(3) hot extrusion
A key character of strengthened dispersion alloy is that work hardening is remarkable, and the processing means that hot extrusion is far longer than other metal working process as a kind of total deformation is applied to Cu-(Al 2o 3+ Y 2o 3) on matrix material, not only greatly can improve material density, and its fracture toughness property can be improved, increase yield strength, improve plasticity and the Young's modulus of material.Because Cu sill sintered compact has the less natural characteristics of shrinking percentage, the Cu-(Al of sintering-internal oxidition state 2o 3+ Y 2o 3) density of matrix material is lower, and in sintered compact, there is the defects such as a large amount of cavities, be therefore necessary that further hot extrusion improves its compactness, improve its intensity, improve plasticity.
Introducing due to oxide particle makes the resistance to deformation of matrix metal increase, and plasticity reduces, and suitably improves extrusion temperature, can improve the plasticity of material, reduces resistance to deformation (squeeze).There are some researches show, extrusion load is with the stepwise varying feature of stroke, and temperature often raises 40 DEG C, and extrusion pressure approximately reduces by 40 ~ 60MPa.Suitable extrusion temperature should be selected for different matrix alloies, extrusion temperature is too high can there is matrix alloy burn-off phenomenon, and due to the reduction of body material plasticity, when the additional potential stress suffered by cladding material reaches the Materials Fracture limit, there is circumferential crack in material surface.Therefore too high extrusion temperature should not be selected.Simultaneously also will for Al 2o 3+ Y 2o 3dispersion-strengthened Cu deformation resistance is high, and the feature that preliminary work hardening rate is high and softening temperature is high is selected.
By certain extrusion ratio, make powder particle bonding state be converted into the DB of metallurgical structure by mechanical bond in guarantee extrusion process, granule boundary disappears, the final performance ensureing material.The dense structure of the large then matrix material of extrusion ratio, even particle distribution, crystal grain are tiny, performance is high.But extrusion ratio is large, and squeeze raises rapidly.There are some researches show, when little extrusion ratio λ is 2.25:1, the mechanical property of matrix material does not improve on the contrary lower than casting state; When extrusion ratio λ is 8:1, density and hardness curve can see respective flex point.Think that 8:1 is the minimum extrusion ratio making this alloy reach " fully " densification, under the condition of large extrusion ratio 10:1, last effect plays a leading role, and after hot extrusion, the mechanical property of matrix material is significantly higher than as cast condition matrix material.
To sum up, the present invention adopts hot extrusion, and extrusion temperature is 900 ~ 1000 DEG C, and extruding rate is 8 ~ 12mms -1, extrusion ratio is not less than 11:1.
(4) cold precision forging
Al 2o 3+ Y 2o 3the important strengthening mechanism of dispersed and strengthened copper-based composite material is exactly the multiple strengthening of working hardening and dispersion-strengthened, and has the excellent specific property its working hardening effect being remained to comparatively high temps, Al 2o 3+ Y 2o 3the use state of dispersed and strengthened copper-based composite material is generally cold deformation state.In addition, for the dispersion-strengthened Cu-(Al prepared by powder metallurgy 2o 3+ Y 2o 3) matrix material, cold deformation can further improve density, improves the performance of this matrix material.Cold roller and deformed can at Al 2o 3+ Y 2o 3particle periphery produces a large amount of dislocation loop group, hinders the slippage of dislocation and climbs, and can keep hardening state and not produce reply, therefore its working hardening effect can be remained to comparatively high temps.Someone have studied Cu-0.9%Al 2o 3powdered alloy is squeezed into bar, and the cold working of shrinking percentage through 80%, it is carried out to the test of hardness, tensile strength and elongation thereupon, finds that tensile strength increases with uniform speed, is approximately that drawing section often shrinks 1% its value and increases 1MPa.Due to the unique effect of working hardening to the strength of materials and the minor impact to specific conductivity, the shaping employing working hardening that material is final, to obtain the overall equilbrium of intensity and electroconductibility.
To sum up, the present invention carries out cold closed-die forging distortion to hot extrusion state matrix material, and deflection elects 60 ~ 80% as.
Beneficial effect of the present invention:
The present invention is with Cu 2o powder and Cu-Al-Y powdered alloy are raw material, dispersion copper matrix material is prepared through batch mixing, compacting, sintering-internal oxidition, extruding, forging, this matrix material has high strength and high conductivity, intensity is at more than 500Pa, and specific conductivity, at more than 80%IACS, overcomes the defect that other composite material high strength degree and high connductivity can not get both, there is excellent softening resistant performance simultaneously, hot strength is high, and plasticity is good, and softening temperature is more than 800 DEG C.This alloy material can be used for the field such as rotor bar, high-thrust rocket liner of the osculatory of electric car and electric locomotive, the conductor material of pulse magnetic field, the electrode of all kinds of spot welding and roll seam welding machine, high-voltage switch gear conducting rod, device for switching resilient material, continuous casting steel machine crystallizer, large high-speed turbo-generator, can improve the quality of products and productivity for the processing enterprise of copper alloy, reduce production cost.
The present invention utilizes metallurgical reaction (melting and powder by atomization process) and internal oxidition two physical processes, two kinds of easy internal oxidition constituent elements, and (oxide structure of the same race is different, as Al to produce mixed structure 2o 3there are α, γ two kinds of structures respectively), the collaborative dispersion-strengthened effect of mixed species oxide compound, improve material property further.In the present invention, the preparation technology of dispersion copper matrix material is reasonable, simple to operate, can ensure quality product, is suitable for large-scale industrial production application.
Embodiment
Following embodiment is only described in further detail the present invention, but does not form any limitation of the invention.
Embodiment 1
Dispersion copper matrix material in the present embodiment, is made up of the component of following mass percent: Al 2o 30.24%, Y 2o 30.16%, surplus is Cu and inevitable impurity.
For the preparation of the powder of dispersion copper matrix material, be made up of the component of following mass percent: 1.58%Cu 2o powder, surplus is Cu-Al-Y powdered alloy; The mass percent that Al and Y accounts for 0.25%, Al and Y of Cu-Al-Y powdered alloy quality is altogether 50%:50%.Cu 2granularity-325 order+400 order of O powder, purity>=99.0%, commercially available.
The preparation method of dispersion copper matrix material, comprises the following steps:
(1) preparation of Cu-Al-Y powdered alloy
Get following raw material: standard cathode copper Cu-CATH-2, Cu content >=99.95wt%; Remelting aluminium ingot Al99.70, Al content >=99.70wt%; Rare earth metal yttrium Y-1, Y content >99.5%; Prepare burden according to following weight proportion: remelting aluminium ingot Al99.70,0.125wt%; Rare earth metal yttrium Y-1,0.125wt%; Surplus is standard cathode copper Cu-CATH-2; Employing protective atmosphere smelting furnace carries out fusing and industrial nitrogen powder by atomization device carries out powder by atomization, and obtained Cu-0.25wt% (Al+Y) powdered alloy, obtains-270 order+400 order Cu-0.25wt% (Al+Y) powdered alloys through screening;
(2) mixing of powder
Cu is got according to mass percent 2o powder 1.58% and Cu-0.25wt% (Al+Y) powdered alloy 98.42%, mix in powder machine in HY-100 type and fully mix 3h;
(3) room temperature isostatic cool pressing compacting
The above-mentioned powder mixed is loaded urethanes mould, adopts LDJm400 type cold isostatic press to carry out the compacting of room temperature isostatic cool pressing, pressure 270MPa, pressing speed 40MPa/min, pressurize 10min, finally obtain the cylindrical billet of Φ 50mm × 200mm;
(4) sintering-internal oxidition
By the billet after shaping, put into Q235 steel sealing container, around billet, add the fresh carburizing agent of thick 5mm as antioxidant, to absorb the oxygen in container, prevent material oxidized, after refractory mortar good seal, put into JR-1300 type high temperature resistance furnace and carry out sintering-internal oxidition comprehensive treating process, sintering-internal oxidition temperature is 950 DEG C, heat up with stove, soaking time 8 hours, after insulation terminates, be cooled to less than 100 DEG C, take out billet;
(5) hot extrusion
Sintered ingot is directly loaded temperature is 1000 DEG C, heat in XJ-1000 type high temperature resistance furnace and be incubated 1.0 hours, put into rapidly the hot-extrusion mold extruding be arranged on XJ-500 copper extruder again, the demoulding, from the bottom of die, extruded rod is ejected, complete extruding, extrusion ratio is 12:1, and extruding rate is 10mms -1, the diameter of rod after extruding is 12.5mm;
(6) cold precision forging
Bar after hot extrusion is carried out cutting stock according to electrical contact accessory size, cold precision forging, cold plastic deformation amount is 60%;
Prepared Cu-(Al 2o 3+ Y 2o 3) dispersion copper matrix material electrical contact, its intensity is 535MPa, and specific conductivity is 90%IACS, and softening temperature is 880 DEG C.
Embodiment 2
Dispersion copper matrix material in the present embodiment is made up of the component of following mass percent: Al 2o 31.02%, Y 2o 30.076%, surplus is Cu and inevitable impurity.
For the preparation of the powder of dispersion copper matrix material, be made up of the component of following mass percent: 5.33%Cu 2o powder, surplus is Cu-Al-Y powdered alloy; The mass percent that Al and Y accounts for 0.60%, Al and Y of Cu-Al-Y powdered alloy quality is altogether 90%:10%.Cu 2granularity-325 order+400 order of O powder, purity>=99.0%, commercially available.
The preparation method of dispersion copper matrix material, comprises the following steps:
(1) preparation of Cu-Al-Y powdered alloy
Get following raw material: standard cathode copper Cu-CATH-2, Cu content >=99.95wt%; Remelting aluminium ingot Al99.70, Al content >=99.70wt%; Rare earth metal yttrium Y-1, Y content >99.5%; Prepare burden according to following weight proportion: remelting aluminium ingot Al99.70,0.54wt%; Rare earth metal yttrium Y-1,0.06wt%; Surplus is standard cathode copper Cu-CATH-2; Employing protective atmosphere smelting furnace carries out fusing and industrial nitrogen powder by atomization device carries out powder by atomization, and obtained Cu-0.60wt% (Al+Y) powdered alloy, obtains-270 order+400 order Cu-0.60wt% (Al+Y) powdered alloys through screening;
(2) mixing of powder
Cu is got according to mass percent 2o powder 5.33% and Cu-0.60wt% (Al+Y) powdered alloy 94.67%, mix in powder machine in HY-100 type and fully mix 3h;
(3) room temperature isostatic cool pressing compacting
The above-mentioned powder mixed is loaded urethanes mould, adopts LDJm400 type cold isostatic press to carry out the compacting of room temperature isostatic cool pressing, pressure 350MPa, pressing speed 60MPa/min, pressurize 6min, finally obtain the cylindrical billet of Φ 75mm × 280mm;
(4) sintering-internal oxidition
By the billet after shaping, put into Q235 steel sealing container, around billet, add the fresh carburizing agent of thick 5mm as antioxidant, after refractory mortar good seal, put into JR-1300 type high temperature resistance furnace and carry out sintering-internal oxidition comprehensive treating process, sintering-internal oxidition temperature is 975 DEG C, heat up with stove, soaking time 6 hours, after insulation terminates, be cooled to less than 100 DEG C, take out billet;
(5) hot extrusion
Sintered ingot is directly loaded temperature is 950 DEG C, heat in XJ-1000 type high temperature resistance furnace and be incubated 1.5 hours, put into rapidly the hot-extrusion mold extruding be arranged on XJ-500 copper extruder again, the demoulding, from the bottom of die, extruded rod is ejected, complete extruding, extrusion ratio is 11:1, and extruding rate is 8mms -1, the diameter of rod after extruding is 19.5mm;
(6) cold precision forging
Bar after hot extrusion is carried out cutting stock according to electrical contact accessory size, cold precision forging, cold plastic deformation amount is 80%.
Prepared Cu-(Al 2o 3+ Y 2o 3) dispersion copper matrix material electrical contact, its intensity is 614MPa, and specific conductivity is 84%IACS, and softening temperature is 930 DEG C.
Embodiment 3
Dispersion copper matrix material in the present embodiment is made up of the component of following mass percent: Al 2o 33.74%, Y 2o 30.03%, surplus is Cu and inevitable impurity.
For the preparation of the powder of dispersion copper matrix material, be made up of the component of following mass percent: 18.96%Cu 2o powder, surplus is Cu-Al-Y powdered alloy; The mass percent that Al and Y accounts for 2.0%, Al and Y of Cu-Al-Y powdered alloy quality is altogether 98%:2%.Cu 2granularity-325 order+400 order of O powder, purity>=99.0%, commercially available.
The preparation method of dispersion copper matrix material, comprises the following steps:
(1) preparation of Cu-Al-Y powdered alloy
Get following raw material: standard cathode copper Cu-CATH-2, Cu content >=99.95wt%; Remelting aluminium ingot Al99.70, Al content >=99.70wt%; Rare earth metal yttrium Y-1, Y content >99.5%; Prepare burden according to following weight proportion: remelting aluminium ingot Al99.70,1.96wt%; Rare earth metal yttrium Y-1,0.04wt%; Surplus is standard cathode copper Cu-CATH-2; Employing protective atmosphere smelting furnace carries out fusing and industrial nitrogen powder by atomization device carries out powder by atomization, and obtained Cu-2.0wt% (Al+Y) powdered alloy, obtains-270 order+400 order Cu-2.0wt% (Al+Y) powdered alloys through screening;
(2) mixing of powder
Cu is got according to mass percent 2o powder 18.96% and Cu-2.0wt% (Al+Y) powdered alloy 81.04%, mix in powder machine in HY-100 type and fully mix 3h;
(3) room temperature isostatic cool pressing compacting
The above-mentioned powder mixed is loaded urethanes mould, adopts LDJm400 type cold isostatic press to carry out the compacting of room temperature isostatic cool pressing, pressure 380MPa, pressing speed 50MPa/min, pressurize 2min, finally obtain the cylindrical billet of Φ 100mm × 300mm;
(4) sintering-internal oxidition
By the billet after shaping, put into Q235 steel sealing container, around billet, add the fresh carburizing agent of thick 5mm as antioxidant, after refractory mortar good seal, put into JR-1300 type high temperature resistance furnace and carry out sintering-internal oxidition comprehensive treating process, sintering-internal oxidition temperature is 1000 DEG C, heat up with stove, soaking time 2 hours, after insulation terminates, be cooled to less than 100 DEG C, take out billet;
(5) hot extrusion
Sintered ingot is directly loaded temperature is 900 DEG C, heat in XJ-1000 type high temperature resistance furnace and be incubated 3.0 hours, put into rapidly the hot-extrusion mold extruding be arranged on XJ-500 copper extruder again, the demoulding, from the bottom of die, extruded rod is ejected, complete extruding, extrusion ratio is 12:1, and extruding rate is 12mms -1, the diameter of rod after extruding is 26.1mm;
(6) cold precision forging
Bar after hot extrusion is carried out cutting stock according to electrical contact accessory size, cold precision forging, cold plastic deformation amount is 70%.
Prepared Cu-(Al 2o 3+ Y 2o 3) dispersion copper matrix material electrical contact, its intensity is 580MPa, and specific conductivity is 80.5%IACS, and softening temperature is 825 DEG C.
Embodiment 4
Dispersion copper matrix material in the present embodiment is made up of the component of following mass percent: Al 2o 32.34%, Y 2o 30.60%, surplus is Cu and inevitable impurity.
For the preparation of the powder of dispersion copper matrix material, be made up of the component of following mass percent: 13.19%Cu 2o powder, surplus is Cu-Al-Y powdered alloy; The mass percent that Al and Y accounts for 1.71%, Al and Y of Cu-Al-Y powdered alloy quality is altogether 74%:26%.Cu 2granularity-325 order+400 order of O powder, purity>=99.0%, commercially available.
The preparation method of dispersion copper matrix material, comprises the following steps:
(1) preparation of Cu-Al-Y powdered alloy
Get following raw material: standard cathode copper Cu-CATH-2, Cu content >=99.95wt%; Remelting aluminium ingot Al99.70, Al content >=99.70wt%; Rare earth metal yttrium Y-1, Y content >99.5%; Prepare burden according to following weight proportion: remelting aluminium ingot Al99.70,0.125wt%; Rare earth metal yttrium Y-1,0.125wt%; Surplus is standard cathode copper Cu-CATH-2; Employing protective atmosphere smelting furnace carries out fusing and industrial nitrogen powder by atomization device carries out powder by atomization, and obtained Cu-1.71wt% (Al+Y) powdered alloy, obtains-270 order+400 order Cu-1.71wt% (Al+Y) powdered alloys through screening;
(2) mixing of powder
Cu is got according to mass percent 2o powder 13.19% and Cu-1.71wt% (Al+Y) powdered alloy 86.81%, mix in powder machine in HY-100 type and fully mix 3h;
(3) room temperature isostatic cool pressing compacting
The above-mentioned powder mixed is loaded urethanes mould, adopts LDJm400 type cold isostatic press to carry out the compacting of room temperature isostatic cool pressing, pressure 270MPa, pressing speed 40MPa/min, pressurize 10min, finally obtain the cylindrical billet of Φ 50mm × 200mm;
(4) sintering-internal oxidition
By the billet after shaping, put into Q235 steel sealing container, around billet, add the fresh carburizing agent of thick 5mm as antioxidant, after refractory mortar good seal, put into JR-1300 type high temperature resistance furnace and carry out sintering-internal oxidition comprehensive treating process, sintering-internal oxidition temperature is 950 DEG C, heat up with stove, soaking time 10 hours, after insulation terminates, be cooled to less than 100 DEG C, take out billet;
(5) hot extrusion
Sintered ingot is directly loaded temperature is 1000 DEG C, heat in XJ-1000 type high temperature resistance furnace and be incubated 1.0 hours, put into rapidly the hot-extrusion mold extruding be arranged on XJ-500 copper extruder again, the demoulding, from the bottom of die, extruded rod is ejected, complete extruding, extrusion ratio is 12:1, and extruding rate is 10mms -1, the diameter of rod after extruding is 12.5mm;
(6) cold precision forging
Bar after hot extrusion is carried out cutting stock according to electrical contact accessory size, cold precision forging, cold plastic deformation amount is 60%.
Prepared Cu-(Al 2o 3+ Y 2o 3) dispersion copper matrix material electrical contact, its intensity is 627MPa, and specific conductivity is 80.5%IACS, and softening temperature is 900 DEG C.
Embodiment 5
Dispersion copper matrix material in the present embodiment is made up of the component of following mass percent: Al 2o 30.65%, Y 2o 31.27%, surplus is Cu and inevitable impurity.
For the preparation of the powder of dispersion copper matrix material, be made up of the component of following mass percent: 6.18%Cu 2o powder, surplus is Cu-Al-Y powdered alloy; The mass percent that Al and Y accounts for 1.34%, Al and Y of Cu-Al-Y powdered alloy quality is altogether 25%:75%.Cu 2granularity-325 order+400 order of O powder, purity>=99.0%, commercially available.
The preparation method of dispersion copper matrix material, comprises the following steps:
(1) preparation of Cu-Al-Y powdered alloy
Get following raw material: standard cathode copper Cu-CATH-2, Cu content >=99.95wt%; Remelting aluminium ingot Al99.70, Al content >=99.70wt%; Rare earth metal yttrium Y-1, Y content >99.5%; Prepare burden according to following weight proportion: remelting aluminium ingot Al99.70,0.54wt%; Rare earth metal yttrium Y-1,0.06wt%; Surplus is standard cathode copper Cu-CATH-2; Employing protective atmosphere smelting furnace carries out fusing and industrial nitrogen powder by atomization device carries out powder by atomization, and obtained Cu-1.34wt% (Al+Y) powdered alloy, obtains-270 order+400 order Cu-1.34wt% (Al+Y) powdered alloys through screening;
(2) mixing of powder
Cu is got according to mass percent 2o powder 6.18% and Cu-1.34wt% (Al+Y) powdered alloy 93.82%, mix in powder machine in HY-100 type and fully mix 3h;
(3) room temperature isostatic cool pressing compacting
The above-mentioned powder mixed is loaded urethanes mould, adopts LDJm400 type cold isostatic press to carry out the compacting of room temperature isostatic cool pressing, pressure 350MPa, pressing speed 60MPa/min, pressurize 6min, finally obtain the cylindrical billet of Φ 75mm × 280mm;
(4) sintering-internal oxidition
By the billet after shaping, put into Q235 steel sealing container, around billet, add the fresh carburizing agent of thick 5mm as antioxidant, after refractory mortar good seal, put into JR-1300 type high temperature resistance furnace and carry out sintering-internal oxidition comprehensive treating process, sintering-internal oxidition temperature is 975 DEG C, heat up with stove, soaking time 8 hours, after insulation terminates, be cooled to less than 100 DEG C, take out billet;
(5) hot extrusion
Sintered ingot is directly loaded temperature is 1000 DEG C, heat in XJ-1000 type high temperature resistance furnace and be incubated 1.5 hours, put into rapidly the hot-extrusion mold extruding be arranged on XJ-500 copper extruder again, the demoulding, from the bottom of die, extruded rod is ejected, complete extruding, extrusion ratio is 11:1, and extruding rate is 8mms -1, the diameter of rod after extruding is 19.5mm;
(6) cold precision forging
Bar after hot extrusion is carried out cutting stock according to electrical contact accessory size, cold precision forging, cold plastic deformation amount is 60%.
Prepared Cu-(Al 2o 3+ Y 2o 3) dispersion copper matrix material electrical contact, its intensity is 591MPa, and specific conductivity is 82%IACS, and softening temperature is 860 DEG C.

Claims (10)

1. dispersion copper matrix material, is characterized in that: be made up of the component of following mass percent: Al 2o 30.24 ~ 3.74%, Y 2o 30.03 ~ 1.27%, surplus is Cu and inevitable impurity.
2. for the preparation of the powder of dispersion copper matrix material, it is characterized in that: be made up of the component of following mass percent: 1.22 ~ 21.79%Cu 2o powder, surplus is Cu-Al-Y powdered alloy; The mass percent that Al and Y accounts for 0.25 ~ 2.0%, Al and Y of Cu-Al-Y powdered alloy quality is altogether (25% ~ 90%): (10% ~ 75%).
3. powder according to claim 2, is characterized in that: be made up of the component of following mass percent: Cu 2o powder 1.58 ~ 18.96%, surplus is Cu-Al-Y powdered alloy.
4. the powder according to any one of claim 2 ~ 3, is characterized in that: described Cu 2the granularity of O powder is-325 order+400 orders.
5. the powder according to any one of claim 2 ~ 3, is characterized in that: the granularity of described Cu-Al-Y powdered alloy is-270 order+400 orders.
6. the preparation method of dispersion copper matrix material, is characterized in that: get the powder according to any one of claim 2 ~ 5, by Cu 2o powder and Cu-Al-Y powdered alloy fully mix rear press forming and obtain billet, and billet is extrusion molding after the process of sintering internal oxidition, and forging, to obtain final product.
7. preparation method according to claim 6, is characterized in that: described in be compressed to room temperature isostatic cool pressing compacting, pressure is 270 ~ 380MPa, and pressing speed is 40 ~ 60MPa/min, and the dwell time is 2 ~ 10min.
8. preparation method according to claim 6, is characterized in that: the temperature of described sintering internal oxidition is 950 ~ 1000 DEG C, and soaking time is 2 ~ 10h.
9. preparation method according to claim 6, is characterized in that: described extruding is hot extrusion, and extrusion temperature is 900 ~ 1000 DEG C, and extruding rate is 8 ~ 12mms -1, extrusion ratio is not less than 11:1.
10. preparation method according to claim 6, is characterized in that: described in be forged to cold closed-die forging distortion, deflection is 60 ~ 80%.
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CN105938763A (en) * 2016-06-21 2016-09-14 哈尔滨东大高新材料股份有限公司 Dispersion-strengthened copper-based contact material added with La2O3-MoSi2, and preparation method of material
CN106191506A (en) * 2016-07-12 2016-12-07 黄天增 A kind of preparation technology of external oxidation dispersion strengthening copper alloy
CN106191506B (en) * 2016-07-12 2017-09-01 黄天增 A kind of preparation technology of external oxidation dispersion strengthening copper alloy
CN106783305A (en) * 2016-12-05 2017-05-31 安徽永川电气设备有限公司 A kind of high-tension switch cabinet static contact method for preparing powder metallurgy
CN107863199A (en) * 2017-10-11 2018-03-30 陕西斯瑞新材料股份有限公司 A kind of preparation method of the copper-clad dispersion copper conducting rod of high-strength highly-conductive high softening temperature
CN108913928A (en) * 2018-05-24 2018-11-30 北京科技大学 A method of preparing oxide dispersion intensifying carbon/carbon-copper composite material
CN112322922A (en) * 2020-11-14 2021-02-05 中国兵器科学研究院宁波分院 Powder metallurgy preparation method of dispersion copper-copper laminated composite material
CN112322922B (en) * 2020-11-14 2022-04-22 中国兵器科学研究院宁波分院 Powder metallurgy preparation method of dispersion copper-copper laminated composite material
CN112786224A (en) * 2020-12-31 2021-05-11 中核北方核燃料元件有限公司 Method for connecting silicon carbide composite fuel cladding and end plug
CN113718127A (en) * 2021-08-16 2021-11-30 安泰科技股份有限公司 High-performance copper-based solid self-lubricating composite material and preparation method thereof
CN113862505A (en) * 2021-09-24 2021-12-31 华中科技大学 Coherent nano oxide dispersion strengthened copper alloy and preparation method and application thereof
CN114959343A (en) * 2022-05-30 2022-08-30 河南科技大学 Forging forming method of aluminum oxide dispersion strengthening copper-based composite material and composite blank
CN114959343B (en) * 2022-05-30 2024-03-29 河南科技大学 Forging forming method of aluminum oxide dispersion strengthening copper-based composite material and composite blank

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