CN105132736B - Disperse carbon/carbon-copper composite material and preparation method thereof - Google Patents
Disperse carbon/carbon-copper composite material and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a kind of disperse carbon/carbon-copper composite material and preparation method thereof, belong to disperse copper processing techniques field.Disperse carbon/carbon-copper composite material is made up of the component of following mass percent：Al2O30.24~3.74%, Y2O30.03~1.27%, surplus is Cu and inevitable impurity.The present invention is with Cu2O powder and Cu Al y alloys powder are raw material, disperse carbon/carbon-copper composite material is prepared through batch mixing, compacting, sintering internal oxidition, extruding, forging, the composite has high intensity and high conductivity, for intensity in more than 500Pa, electrical conductivity overcomes other composite material high strength degree and highly conductive the defects of can not getting both in more than 80%IACS, there is excellent softening resistant performance simultaneously, elevated temperature strength is high, and plasticity is good, and softening temperature is more than 800 DEG C.
Description
Technical field
The present invention relates to a kind of disperse carbon/carbon-copper composite material, the preparation method of disperse carbon/carbon-copper composite material is also related to, is belonged to
Disperse copper processing techniques field.
Background technology
Al as disperse phase2O3Particle is to Cu-Al2O3The contribution of composite material strength is mainly manifested in following side
Face (1) Al2O3Particle pinning dislocation, under certain condition as dislocation source, increase dislocation density；(2)Al2O3The presence of particle
Dislocation, sub boundary motion are hindered, so as to hinder the formation of recrystallization nucleus and crystal grain to grow up；(3)Al2O3The presence of particle can
Suppress static and dynamic recrystallization progress.Therefore, Cu-Al2O3Composite has high thermal conductivity, high conductivity and excellent
The advantages that elevated temperature strength, high-temperature creep resistance, anti-wear performance are good, have in fields such as electromechanics, electronics, aerospace and atomic energy huge
Big application potential, the extensive research interest of people is caused.
The preparation of ODS copper-base alloys, key are how to obtain ultra-fine alumina particle and make its equably disperse point
Cloth improves its mechanical behavior under high temperature on Copper substrate while high conductance is ensured.Conventional preparation method mainly has：Pass
Powder metallurgic method of uniting and improved powder metallurgic method, including mechanical alloying method, coprecipitation, sol-gel process, in-situ reducing
Method etc..Many dispersion-strengthened Cu new preparation technologies are emerged in recent years, such as reactive spray-deposition, vacuum mixing casting, XD methods
With internal oxidation etc., its main purpose is to keep to reduce dispersion-strengthened Cu on the basis of traditional dispersion-strengthened Cu product properties
Production cost, to promote the popularization and application of dispersion-strengthened Cu.Wherein Cu-Al alloy powders internal oxidation is prepared by current commercialization
The Cu-Al of function admirable2O3The optimal path of composite.The Cu-0.7Al prepared such as SCM Corporation of the U.S. with internal oxidation2O3
Composite, tensile strength reaches 585Ma, elongation percentage 11%, electrical conductivity 85%IACS, and has excellent anti-softening temperature
Degree.The country also has many unit research internal oxidations to prepare Cu-Al2O3Cu- prepared by composite, wherein University Of Tianjin
0.62Al2O3Composite, tensile strength reach 608Ma, electrical conductivity 80%IACS.
Traditional internal oxidation prepares Cu-Al2O3The technique of alloy is：First according to Al content require carry out dispensing and
Melting Cu-Al alloys in induction furnace, then using water atomization or N2Cu-Al alloy melts are atomized into Cu-Al alloy powders.Will
Dried Cu-Al alloy powders and Cu2O powder is well mixed, then mixed-powder is put into vacuum drying oven and is heated to 800~
1000 DEG C, held for some time carries out internal oxidition.Control partial pressure of oxygen is oxidized the Al in Cu-Al alloys, and Cu is not oxidized.
Internal oxidition terminates just to obtain Cu-Al2O3The Cu of powder and Cu powder and remnants2O mixed-powder.H is passed through again2Residual oxygen is removed, just
Obtain Cu-Al2O3Powder and Cu powder.Jacket is carried out again, is vacuumized, isostatic pressed base, then hot extrusion, obtains extrusion blank, then
Cold-drawn obtains required section bar.
However, traditional internal oxidation prepares Cu-Al2O3Many problems also be present in composite：(1) process is more, the cycle
Long, production cost is high, it is impossible to manufactures large scale and complex-shaped part；(2) influence factor is too many, and production process is not easily-controllable
System, quality of materials are unstable；(3) automation, scale, continuous production are difficult to, so it is difficult to carrying out popularization and application.With vapour
Exemplified by car welding and assembling production lines spot-wedling electrode, the conventional Cr-Zr-Cu bar costs of spot-wedling electrode are about 60,000 yuan/ton at present, are adopted
The Cu-Al prepared with traditional internal oxidation process2O3The cost of composite is about 150,000 yuan/ton, although Cu-Al2O3Composite
The service life of electrode is more than 3 times of traditional Cr-Zr-Cu electrodes, but cost is also up to 2.5 times, along with using producer
Custom, it is difficult to carry out popularization and application.This is also current Cu-Al2O3The subject matter faced in composite popularization and application.Cause
This, designs new dispersion copper contact material, develops new technology of preparing to simplify technique, reduce cost, raising efficiency, expansion life
Production scale, turn into a highly important task.
Publication number CN101338389A patent of invention discloses a kind of integral dispersion copper rare-earth copper alloy material
And the preparation method of dispersion copper, rare-earth copper alloy material are mainly comprising Cu, Al and rare earth addition RE, each component content：Al
0.05~0.5wt% of 0.1~1wt%, RE, surplus Cu, its middle rare earth RE refer to Y or Ce or mixed rare-earth elements (Ce+Y).
The preparation method of dispersion copper includes：1) melting of alloy：Heat up refining after Cu-CATH-1 (purity 99.95%) is melted, then
Al insulation meltings are added, Y is added under Ar gas shieldeds, is cast after being sufficiently stirred, cooling is come out of the stove；2) hot-working of alloy：In temperature
The insulation 4~8 hours of 850~950 DEG C of degree carries out hot extrusion or hot rolling；3) solid solution of alloy：The temperature of solution treatment is 900
~950 DEG C, soaking time 2~4 hours, the laggard water-filling of solution treatment is quenched；4) cold deformation：Shunting time drawing process.The party
Dispersion copper prepared by method has the characteristics that high strength ＆ high electric-conduction, high anti-softening temperature, but its intensity and conductance still need
Improve.
The content of the invention
It is an object of the invention to provide a kind of dispersion copper with high intensity, high conductivity and good mechanical behavior under high temperature to answer
Condensation material.
Meanwhile the present invention also provides a kind of preparation method of disperse carbon/carbon-copper composite material.
In order to realize the above object the technical solution adopted in the present invention is：
Disperse carbon/carbon-copper composite material, it is made up of the component of following mass percent：Al2O30.24~3.74%, Y2O30.03~
1.27%, surplus is Cu and inevitable impurity.
For preparing the powder of disperse carbon/carbon-copper composite material, it is made up of the component of following mass percent：1.22~21.79%
Cu2O powder, surplus are Cu-Al-Y alloy powders；Preferably, Cu2O powder 1.58~18.96%, surplus are Cu-Al-Y alloys
Powder.Al and Y account for altogether 0.25~2.0%, the Al and Y of Cu-Al-Y alloy powder quality mass percent for (25%~
90%):(10%~75%).Cu2O addition is generally the 120% of requisite oxygen, and unnecessary oxygen can be escaped in high temperature by assembling
Go out, only very small amount can exist in the form of CuAlO compounds, influence very little to conductance, intensity rises on the contrary.
The Cu2The granularity of O powder is the mesh of -325 mesh+400 (can by 325 mesh but can not be by 400 mesh), purity >=
99.0%.
The granularity of the Cu-Al-Y alloy powders is that the mesh of -270 mesh+400 (by 270 mesh but can not pass through 400
Mesh).It is made by raw material Cu, Al, Y through melting, powder by atomization technique.Standard cathode copper Cu-CATH-2, Cu can be selected in raw material Cu
Content >=99.95wt%；Remelting aluminium ingot Al 99.70, Al content >=99.70wt% can be selected in Al；Rare earth metal can be selected in Y
Yttrium Y-1, Y content>99.5%.
In the present invention, Rare Earth Y mainly have of both act on, when micro Y purify in alloy melting melt and carefully
Change crystal grain, high-melting-point Y is generated by metallurgical reaction2O3Forming core crystal grain thinning and second-phase dispersion is promoted to strengthen, second, by additional
Unoxidized Y in alloy internal oxidition reaction and is formed in situ and the compact nanometer Y of matrix by oxidant occurs2O3, with internal oxidition
Caused Al2O3Collective effect, to produce the dispersion-strengtherning effect for mixing type of metal oxide.Also, Al, the Y added exists
More stable oxide structure can be produced in atomization process by metallurgical reaction, such as produces α-Al2O3, different from only occurring
γ-Al caused by internal oxidition2O3。
Research shows, in the preparation process of Cu-Al-Y alloy powders, either water atomization or general industry nitrogen mist
Change, do not dissolve in the nonmetallic compound of acid in prepared Cu-Al-Y alloy powders always by metallurgical reaction generation small part,
XRD analysis are shown to be α-Al2O3And Y2O3.Therefore, the oxide dispersion intensifying copper prepared by atomization and internal oxidition, its oxygen
The source of compound is different, and structure is different, and corresponding strengthening mechanism also differs.
With Cu2O powder carries out internal oxidition after making the Cu-Al-Y mixed powder for alloy compacting of oxygen source, in certain temperature and
Under atmosphere, Cu2O resolves into Cu and [O]；[O] is adsorbed and is dissolved in Cu-Al-Y alloying pellets surface；[O] matrix Cu spread and with
Al preferential oxidations are into Al in matrix2O3, internal oxidition is completed, obtains the Cu- (Al of dispersion-strengtherning2O3+Y2O3) composite.In this mistake
Cheng Zhong, because the diffusion coefficient of [O] in copper is far longer than the diffusion coefficient of Al and Y in copper, it can be considered that being in situ
Generate Al2O3+Y2O3。
Carry out oxidant Cu2When O content selects, it is contemplated that following factor：(1) phosphorus etc. is contained in Cu-Al-Y alloy powders
Impurity element, the element such as order arrangement, P, Al, As, Fe, Ni, Mg, Sn, Si and Zn with copper if forming solid solution by size
The electrical conductivity of copper alloy can be greatly reduced, therefore as far as possible to be aoxidized impurity element；(2) Cu as oxygen source2O high temperature
Cu-Al-Y alloy powders surface can not possibly be adsorbed in after decomposition completely and completes to spread；(3) actual mechanical process can not possibly be as reason
Various parameters are so accurately controlled by calculating.
The preparation method of disperse carbon/carbon-copper composite material is：By Cu2O powder and Cu-Al-Y alloy powders are suppressed after being sufficiently mixed
Billet is shaped to obtain, extrusion molding after the sintered internal oxidition processing of billet, forging, is produced.
(1) compacting of alloy powder
Tradition compacting when, under the pressure of stamping, mixed-powder show to a certain extent with property as liquid phase,
Flowed to all directions, so as to produce lateral pressure to pressing mold wall.But due to intergranular friction, wedging and other factors, make
The transmission that pressure is obtained in sidewall direction is more much smaller than the transmission in pressing direction.Frictional force is produced 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.Pressure distribution
Inhomogeneities the consistency for causing pressed compact each several part is also uneven.The Density Distribution of blank can be improved using isostatic cool pressing
Uniformity and consistency.
If kept for certain time under a certain specific pressure, extraordinary effect can be often obtained.The original of pressurize
Because being：(1) make pressure transmission abundant, be advantageous to the Density Distribution of each several part in pressed compact；(2) air in body of powder hole is made
There is time enough effusion；(3) mechanical engagement and deformation time given between powder, is advantageous to the progress of strain relaxation.
The Frotteurism and work-hardening capacity that pressing speed in pressing process is not only had influence between powder particle, and
Air is had influence on from the interpore effusion situation of powder particle.If pressing speed is too fast, air effusion is just difficult, makes in pressed compact
The defects of increase.Therefore, the pressing process such as cold should be carried out with slow pressurized state.
To sum up, the present invention is suppressed using room temperature isostatic cool pressing, and pressure be 270~380MPa, pressing speed for 40~
60MPa/min (is typically carried in 2~3min and completed), and the dwell time is 2~10min.
(2) sintering-internal oxidition of powder
Because Al, the diffusion of [O] and chemical reaction velocity are in exponential increase with the raising of temperature, therefore, improve
Internal oxidition temperature can be greatly shortened the time required to completing internal oxidition, but during more than 1000 DEG C internal oxiditions, hardness number substantially drops
Low, this is relevant with growing up for particle.Therefore internal oxidition temperature is unsuitable too high, is typically not to be exceeded 1000 DEG C.Internal oxidition is mainly sent out
In raw a period of time shorter in the early stage, with the extension of time, Internal oxidation rate drastically declines, and the actual internal oxidition time is unsuitable
It is long.
To sum up, the temperature of sintering-internal oxidition is 950~1000 DEG C in the present invention, and soaking time is 2~10h.
(3) hot extrusion
One key character of strengthened dispersion alloy is that processing hardening is notable, and hot extrusion is much big as a kind of total deformation
Cu- (Al are applied in the manufacturing process of other metal working process2O3+Y2O3) on composite, it can not only greatly improve material
Expect consistency, and its fracture toughness can be improved, increase yield strength, improve the plasticity and modulus of elasticity of material.Due to Cu
Sill sintered body has the less inherent characteristic of shrinkage factor, the Cu- (Al of sintering-internal oxidition state2O3+Y2O3) composite
Consistency is relatively low, and the defects of substantial amounts of empty in sintered body be present, it is therefore necessary to and further hot extrusion improves its compactness,
Its intensity is improved, improves plasticity.
Because the introducing of oxide particle increases the resistance of deformation of parent metal, plasticity reduces, and suitably improves extruding
Temperature, the plasticity of material can be improved, reduce resistance of deformation (extruding force).There are some researches show extrusion load is with stroke in stage
Variation characteristic, temperature often raise 40 DEG C, and extrusion pressure about reduces by 40~60MPa.It should be selected for different matrix alloys
Appropriate extrusion temperature, extrusion temperature is too high to occur matrix alloy burn-off phenomenon, and because matrix material plasticity reduces, when outer
When additional tension suffered by layer material reaches the Materials Fracture limit, there is circumferential crack in material surface.Therefore should not select
High extrusion temperature.Also to be directed to Al simultaneously2O3+Y2O3Dispersion-strengthened Cu deformation resistance is high, and preliminary work hardening rate is high and softening is warm
Spending the characteristics of high is selected.
By certain extrusion ratio, just can guarantee that in extrusion process makes powder particle bonding state be converted into by mechanical bond
The dense body of metallurgical structure, granule boundary disappear, the final performance for ensureing material.The tissue of the big then composite of extrusion ratio causes
Close, even particle distribution, crystal grain are tiny, performance is high.But extrusion ratio is big, extruding force raises rapidly.There are some researches show small extrusion ratio
λ is 2.25:When 1, the mechanical property of composite is not improved on the contrary less than casting state；Extrusion ratio λ is 8:When 1, in density and
Respective flex point can be seen on hardness curve.Think 8:1 is the minimum extrusion ratio for making the alloy reach " abundant " densification, greatly
Extrusion ratio 10:Under conditions of 1, previous effect plays a leading role, and the mechanical property of composite is significantly higher than as cast condition after hot extrusion
Composite.
To sum up, the present invention uses hot extrusion, and extrusion temperature is 900~1000 DEG C, and extruding rate is 8~12mms-1, squeeze
Pressure ratio is not less than 11:1.
(4) cold precision forging
Al2O3+Y2O3The important strengthening mechanism of dispersed and strengthened copper-based composite material is exactly the comprehensive of working hardening and dispersion-strengtherning
Close and strengthen, and with the excellent specific property that its working hardening effect is remained to higher temperature, Al2O3+Y2O3It is dispersion strengthening copper-based multiple
The use state of condensation material is typically cold deformation state.In addition, for the dispersion-strengtherning Cu- (Al prepared by powder metallurgy2O3+
Y2O3) composite, cold deformation can further improve consistency, improves the performance of the composite.Cold-rolling deformation can be
Al2O3+Y2O3Particle periphery produces a large amount of dislocation ring groups, hinders the sliding of dislocation with climbing, and can keep hardening state without producing
It is raw to reply, therefore its working hardening effect can be remained to higher temperature.Someone have studied Cu-0.9%Al2O3Alloy powder squeezes
Bar is pressed into, and through the cold working of 80% shrinkage factor, carries out the experiment of hardness, tensile strength and elongation, hair to it therewith
Existing tensile strength is increased with uniform speed, and about drawing section often shrinks 1% its value increase 1MPa.Due to working hardening pair
The unique effect of the strength of materials and the minor impact to electrical conductivity, the final shaping of material use working hardening, strong to obtain
The overall balance of degree and electric conductivity.
To sum up, the present invention carries out cold closed-die forging deformation to hot extrusion state composite, and deflection elects 60~80% as.
Beneficial effects of the present invention：
The present invention is with Cu2O powder and Cu-Al-Y alloy powders are raw material, through batch mixing, compacting, sintering-internal oxidition, extruding,
Forging prepares disperse carbon/carbon-copper composite material, and the composite has high intensity and high conductivity, and intensity is in more than 500Pa, electrical conductivity
In more than 80%IACS, other composite material high strength degree and highly conductive the defects of can not getting both are overcome, while have excellent
Softening resistant performance, elevated temperature strength is high, and plasticity is good, and softening temperature is more than 800 DEG C.The alloy material can be used for electric car and electric power machine
The contact line of car, the conductor material of pulse magnetic field, the electrode of all kinds of spot welding and seam welder, high-voltage switch gear conducting rod, switch electricity
Device elastomeric material, continuous casting steel machine crystallizer, the rotor bar of large high-speed turbogenerator, high-thrust rocket liner etc.
Field, it can be that product quality and productivity ratio improve in the processing enterprise of copper alloy, reduce production cost.
The present invention utilizes metallurgical reaction (melting and powder by atomization process) and two physical processes of internal oxidition, two kinds of easily interior oxygen
Change constituent element, producing mixed structure, (oxide structure of the same race is different, such as Al2O3There are two kinds of structures of α, γ respectively), mixed species oxygen
The collaboration dispersion-strengtherning effect of compound, further improves material property.The preparation technology of disperse carbon/carbon-copper composite material closes in the present invention
Reason, it is simple to operate, product quality can be ensured, suitable for large-scale industrial production application.
Embodiment
Following embodiments are only described in further detail to the present invention, but do not form any limitation of the invention.
Embodiment 1
Disperse carbon/carbon-copper composite material in the present embodiment, is made up of the component of following mass percent：Al2O30.24%,
Y2O30.16%, surplus is Cu and inevitable impurity.
For preparing the powder of disperse carbon/carbon-copper composite material, it is made up of the component of following mass percent：1.58%Cu2O powder
End, surplus are Cu-Al-Y alloy powders；Al and Y accounts for 0.25%, the Al and Y of Cu-Al-Y alloy powder quality quality percentage altogether
Than for 50%:50%.Cu2The mesh of the mesh of granularity -325+400 of O powder, purity >=99.0% are commercially available.
The preparation method of disperse carbon/carbon-copper composite material, comprises the following steps：
(1) preparation of Cu-Al-Y alloy powders
Take following raw material：Standard cathode copper Cu-CATH-2, Cu content >=99.95wt%；Remelting aluminium ingot Al 99.70,
Al content >=99.70wt%；Rare earth metal yttrium Y-1, Y content>99.5%；Dispensing is carried out according to following weight proportion：Remelting is used
Aluminium ingot Al 99.70,0.125wt%；Rare earth metal yttrium Y-1,0.125wt%；Surplus is standard cathode copper Cu-CATH-2；Using
Protective atmosphere smelting furnace carries out fusing and industrial nitrogen powder by atomization device carries out powder by atomization, and Cu-0.25wt% (Al+ are made
Y) alloy powder, it is screened to obtain -270 mesh+400 mesh Cu-0.25wt% (Al+Y) alloy powder；
(2) mixing of powder
Cu is taken according to mass percent2O powder 1.58% and Cu-0.25wt% (Al+Y) alloy powder 98.42%,
HY-100 types mix in powder machine and are sufficiently mixed 3h；
(3) room temperature isostatic cool pressing is suppressed
Above-mentioned well mixed powder is loaded into polyurethane rubber mould, room is carried out using LDJm400 types cold isostatic press
Warm isostatic cool pressing compacting, pressure 270MPa, pressing speed 40MPa/min, pressurize 10min, finally gives Φ 50mm × 200mm's
Cylindrical billet；
(4) sintering-internal oxidition
The billet after shaping is put into Q235 steel sealing containers, thick 5mm fresh carburizer is added around billet
As antioxidant, to absorb the oxygen in container, prevent material to be oxidized, after fire clay good seal, be put into JR-1300 types height
- internal oxidition integrated treatment is sintered in warm resistance furnace, sintering-internal oxidition temperature is 950 DEG C, is heated up with stove, soaking time 8 is small
When, after insulation terminates, less than 100 DEG C are cooled to, takes out billet；
(5) hot extrusion
Sintered ingot is directly loadable into temperature to be heated in 1000 DEG C, XJ-1000 type high temperature resistance furnaces and being incubated 1.0 hours,
It is put into rapidly in the hot-extrusion mold on XJ-500 copper extruders and extrudes again, be stripped, will be extruded from the bottom of cavity plate
Rod ejects, and completes extruding, extrusion ratio 12:1, extruding rate 10mms-1, the diameter of rod after extruding is 12.5mm；
(6) cold precision forging
Bar after hot extrusion is subjected to cutting stock, cold precision forging, cold plastic deformation according to electrical contact accessory size
Measure as 60%；
Prepared Cu- (Al2O3+Y2O3) disperse carbon/carbon-copper composite material electrical contact, its intensity is 535MPa, and electrical conductivity is
90%IACS, softening temperature are 880 DEG C.
Embodiment 2
Disperse carbon/carbon-copper composite material in the present embodiment is made up of the component of following mass percent：Al2O31.02%, Y2O3
0.076%, surplus is Cu and inevitable impurity.
For preparing the powder of disperse carbon/carbon-copper composite material, it is made up of the component of following mass percent：5.33%Cu2O powder
End, surplus are Cu-Al-Y alloy powders；Al and Y accounts for 0.60%, the Al and Y of Cu-Al-Y alloy powder quality quality percentage altogether
Than for 90%:10%.Cu2The mesh of the mesh of granularity -325+400 of O powder, purity >=99.0% are commercially available.
The preparation method of disperse carbon/carbon-copper composite material, comprises the following steps：
(1) preparation of Cu-Al-Y alloy powders
Take following raw material：Standard cathode copper Cu-CATH-2, Cu content >=99.95wt%；Remelting aluminium ingot Al 99.70,
Al content >=99.70wt%；Rare earth metal yttrium Y-1, Y content>99.5%；Dispensing is carried out according to following weight proportion：Remelting is used
Aluminium ingot Al 99.70,0.54wt%；Rare earth metal yttrium Y-1,0.06wt%；Surplus is standard cathode copper Cu-CATH-2；Using guarantor
Shield atmosphere smelting furnace carries out fusing and industrial nitrogen powder by atomization device carries out powder by atomization, and Cu-0.60wt% (Al+Y) is made
Alloy powder, it is screened to obtain -270 mesh+400 mesh Cu-0.60wt% (Al+Y) alloy powder；
(2) mixing of powder
Cu is taken according to mass percent2O powder 5.33% and Cu-0.60wt% (Al+Y) alloy powder 94.67%,
HY-100 types mix in powder machine and are sufficiently mixed 3h；
(3) room temperature isostatic cool pressing is suppressed
Above-mentioned well mixed powder is loaded into polyurethane rubber mould, room is carried out using LDJm400 types cold isostatic press
Warm isostatic cool pressing compacting, pressure 350MPa, pressing speed 60MPa/min, pressurize 6min, finally gives Φ 75mm × 280mm's
Cylindrical billet；
(4) sintering-internal oxidition
The billet after shaping is put into Q235 steel sealing containers, thick 5mm fresh carburizer is added around billet
As antioxidant, after fire clay good seal, it is put into JR-1300 type high temperature resistance furnaces and is sintered-internal oxidition integrated treatment,
Sintering-internal oxidition temperature is 975 DEG C, is heated up with stove, soaking time 6 hours, after insulation terminates, is cooled to less than 100 DEG C, takes out
Billet；
(5) hot extrusion
Sintered ingot is directly loadable into temperature to be heated in 950 DEG C, XJ-1000 type high temperature resistance furnaces and being incubated 1.5 hours, then
Rapid be put into the hot-extrusion mold on XJ-500 copper extruders extrudes, and is stripped, from the bottom of cavity plate by extruded rod
Ejection, complete extruding, extrusion ratio 11:1, extruding rate 8mms-1, the diameter of rod after extruding is 19.5mm；
(6) cold precision forging
Bar after hot extrusion is subjected to cutting stock, cold precision forging, cold plastic deformation according to electrical contact accessory size
Measure as 80%.
Prepared Cu- (Al2O3+Y2O3) disperse carbon/carbon-copper composite material electrical contact, its intensity is 614MPa, and electrical conductivity is
84%IACS, softening temperature are 930 DEG C.
Embodiment 3
Disperse carbon/carbon-copper composite material in the present embodiment is made up of the component of following mass percent：Al2O33.74%, Y2O3
0.03%, surplus is Cu and inevitable impurity.
For preparing the powder of disperse carbon/carbon-copper composite material, it is made up of the component of following mass percent：18.96%Cu2O powder
End, surplus are Cu-Al-Y alloy powders；Al and Y accounts for 2.0%, the Al and Y of Cu-Al-Y alloy powder quality quality percentage altogether
Than for 98%:2%.Cu2The mesh of the mesh of granularity -325+400 of O powder, purity >=99.0% are commercially available.
The preparation method of disperse carbon/carbon-copper composite material, comprises the following steps：
(1) preparation of Cu-Al-Y alloy powders
Take following raw material：Standard cathode copper Cu-CATH-2, Cu content >=99.95wt%；Remelting aluminium ingot Al 99.70,
Al content >=99.70wt%；Rare earth metal yttrium Y-1, Y content>99.5%；Dispensing is carried out according to following weight proportion：Remelting is used
Aluminium ingot Al 99.70,1.96wt%；Rare earth metal yttrium Y-1,0.04wt%；Surplus is standard cathode copper Cu-CATH-2；Using guarantor
Shield atmosphere smelting furnace carries out fusing and industrial nitrogen powder by atomization device carries out powder by atomization, and Cu-2.0wt% (Al+Y) is made and closes
Bronze end, it is screened to obtain -270 mesh+400 mesh Cu-2.0wt% (Al+Y) alloy powder；
(2) mixing of powder
Cu is taken according to mass percent2O powder 18.96% and Cu-2.0wt% (Al+Y) alloy powder 81.04%,
HY-100 types mix in powder machine and are sufficiently mixed 3h；
(3) room temperature isostatic cool pressing is suppressed
Above-mentioned well mixed powder is loaded into polyurethane rubber mould, room is carried out using LDJm400 types cold isostatic press
Warm isostatic cool pressing compacting, pressure 380MPa, pressing speed 50MPa/min, pressurize 2min, finally gives Φ 100mm × 300mm's
Cylindrical billet；
(4) sintering-internal oxidition
The billet after shaping is put into Q235 steel sealing containers, thick 5mm fresh carburizer is added around billet
As antioxidant, after fire clay good seal, it is put into JR-1300 type high temperature resistance furnaces and is sintered-internal oxidition integrated treatment,
Sintering-internal oxidition temperature is 1000 DEG C, is heated up with stove, soaking time 2 hours, after insulation terminates, is cooled to less than 100 DEG C, takes
Go out billet；
(5) hot extrusion
Sintered ingot is directly loadable into temperature to be heated in 900 DEG C, XJ-1000 type high temperature resistance furnaces and being incubated 3.0 hours, then
Rapid be put into the hot-extrusion mold on XJ-500 copper extruders extrudes, and is stripped, from the bottom of cavity plate by extruded rod
Ejection, complete extruding, extrusion ratio 12:1, extruding rate 12mms-1, the diameter of rod after extruding is 26.1mm；
(6) cold precision forging
Bar after hot extrusion is subjected to cutting stock, cold precision forging, cold plastic deformation according to electrical contact accessory size
Measure as 70%.
Prepared Cu- (Al2O3+Y2O3) disperse carbon/carbon-copper composite material electrical contact, its intensity is 580MPa, and electrical conductivity is
80.5%IACS, softening temperature are 825 DEG C.
Embodiment 4
Disperse carbon/carbon-copper composite material in the present embodiment is made up of the component of following mass percent：Al2O32.34%, Y2O3
0.60%, surplus is Cu and inevitable impurity.
For preparing the powder of disperse carbon/carbon-copper composite material, it is made up of the component of following mass percent：13.19%Cu2O powder
End, surplus are Cu-Al-Y alloy powders；Al and Y accounts for 1.71%, the Al and Y of Cu-Al-Y alloy powder quality quality percentage altogether
Than for 74%:26%.Cu2The mesh of the mesh of granularity -325+400 of O powder, purity >=99.0% are commercially available.
The preparation method of disperse carbon/carbon-copper composite material, comprises the following steps：
(1) preparation of Cu-Al-Y alloy powders
Take following raw material：Standard cathode copper Cu-CATH-2, Cu content >=99.95wt%；Remelting aluminium ingot Al 99.70,
Al content >=99.70wt%；Rare earth metal yttrium Y-1, Y content>99.5%；Dispensing is carried out according to following weight proportion：Remelting is used
Aluminium ingot Al 99.70,0.125wt%；Rare earth metal yttrium Y-1,0.125wt%；Surplus is standard cathode copper Cu-CATH-2；Using
Protective atmosphere smelting furnace carries out fusing and industrial nitrogen powder by atomization device carries out powder by atomization, and Cu-1.71wt% (Al+ are made
Y) alloy powder, it is screened to obtain -270 mesh+400 mesh Cu-1.71wt% (Al+Y) alloy powder；
(2) mixing of powder
Cu is taken according to mass percent2O powder 13.19% and Cu-1.71wt% (Al+Y) alloy powder 86.81%,
HY-100 types mix in powder machine and are sufficiently mixed 3h；
(3) room temperature isostatic cool pressing is suppressed
Above-mentioned well mixed powder is loaded into polyurethane rubber mould, room is carried out using LDJm400 types cold isostatic press
Warm isostatic cool pressing compacting, pressure 270MPa, pressing speed 40MPa/min, pressurize 10min, finally gives Φ 50mm × 200mm's
Cylindrical billet；
(4) sintering-internal oxidition
The billet after shaping is put into Q235 steel sealing containers, thick 5mm fresh carburizer is added around billet
As antioxidant, after fire clay good seal, it is put into JR-1300 type high temperature resistance furnaces and is sintered-internal oxidition integrated treatment,
Sintering-internal oxidition temperature is 950 DEG C, is heated up with stove, soaking time 10 hours, after insulation terminates, is cooled to less than 100 DEG C, takes
Go out billet；
(5) hot extrusion
Sintered ingot is directly loadable into temperature to be heated in 1000 DEG C, XJ-1000 type high temperature resistance furnaces and being incubated 1.0 hours,
It is put into rapidly in the hot-extrusion mold on XJ-500 copper extruders and extrudes again, be stripped, will be extruded from the bottom of cavity plate
Rod ejects, and completes extruding, extrusion ratio 12:1, extruding rate 10mms-1, the diameter of rod after extruding is 12.5mm；
(6) cold precision forging
Bar after hot extrusion is subjected to cutting stock, cold precision forging, cold plastic deformation according to electrical contact accessory size
Measure as 60%.
Prepared Cu- (Al2O3+Y2O3) disperse carbon/carbon-copper composite material electrical contact, its intensity is 627MPa, and electrical conductivity is
80.5%IACS, softening temperature are 900 DEG C.
Embodiment 5
Disperse carbon/carbon-copper composite material in the present embodiment is made up of the component of following mass percent：Al2O30.65%, Y2O3
1.27%, surplus is Cu and inevitable impurity.
For preparing the powder of disperse carbon/carbon-copper composite material, it is made up of the component of following mass percent：6.18%Cu2O powder
End, surplus are Cu-Al-Y alloy powders；Al and Y accounts for 1.34%, the Al and Y of Cu-Al-Y alloy powder quality quality percentage altogether
Than for 25%:75%.Cu2The mesh of the mesh of granularity -325+400 of O powder, purity >=99.0% are commercially available.
The preparation method of disperse carbon/carbon-copper composite material, comprises the following steps：
(1) preparation of Cu-Al-Y alloy powders
Take following raw material：Standard cathode copper Cu-CATH-2, Cu content >=99.95wt%；Remelting aluminium ingot Al 99.70,
Al content >=99.70wt%；Rare earth metal yttrium Y-1, Y content>99.5%；Dispensing is carried out according to following weight proportion：Remelting is used
Aluminium ingot Al 99.70,0.54wt%；Rare earth metal yttrium Y-1,0.06wt%；Surplus is standard cathode copper Cu-CATH-2；Using guarantor
Shield atmosphere smelting furnace carries out fusing and industrial nitrogen powder by atomization device carries out powder by atomization, and Cu-1.34wt% (Al+Y) is made
Alloy powder, it is screened to obtain -270 mesh+400 mesh Cu-1.34wt% (Al+Y) alloy powder；
(2) mixing of powder
Cu is taken according to mass percent2O powder 6.18% and Cu-1.34wt% (Al+Y) alloy powder 93.82%,
HY-100 types mix in powder machine and are sufficiently mixed 3h；
(3) room temperature isostatic cool pressing is suppressed
Above-mentioned well mixed powder is loaded into polyurethane rubber mould, room is carried out using LDJm400 types cold isostatic press
Warm isostatic cool pressing compacting, pressure 350MPa, pressing speed 60MPa/min, pressurize 6min, finally gives Φ 75mm × 280mm's
Cylindrical billet；
(4) sintering-internal oxidition
The billet after shaping is put into Q235 steel sealing containers, thick 5mm fresh carburizer is added around billet
As antioxidant, after fire clay good seal, it is put into JR-1300 type high temperature resistance furnaces and is sintered-internal oxidition integrated treatment,
Sintering-internal oxidition temperature is 975 DEG C, is heated up with stove, soaking time 8 hours, after insulation terminates, is cooled to less than 100 DEG C, takes out
Billet；
(5) hot extrusion
Sintered ingot is directly loadable into temperature to be heated in 1000 DEG C, XJ-1000 type high temperature resistance furnaces and being incubated 1.5 hours,
It is put into rapidly in the hot-extrusion mold on XJ-500 copper extruders and extrudes again, be stripped, will be extruded from the bottom of cavity plate
Rod ejects, and completes extruding, extrusion ratio 11:1, extruding rate 8mms-1, the diameter of rod after extruding is 19.5mm；
(6) cold precision forging
Bar after hot extrusion is subjected to cutting stock, cold precision forging, cold plastic deformation according to electrical contact accessory size
Measure as 60%.
Prepared Cu- (Al2O3+Y2O3) disperse carbon/carbon-copper composite material electrical contact, its intensity is 591MPa, and electrical conductivity is
82%IACS, softening temperature are 860 DEG C.
Claims (3)
1. disperse carbon/carbon-copper composite material, it is characterised in that：It is made up of the component of following mass percent：1.22~21.79% Cu2O powder
End, surplus are Cu-Al-Y alloy powders；Al and Y accounts for 0.25 ~ 2.0%, the Al and Y of Cu-Al-Y alloy powder quality quality altogether
Percentage is（25%~90%）:（10%~75%）；
The Cu2The granularity of O powder is the mesh of -325 mesh+400；
The granularity of the Cu-Al-Y alloy powders is the mesh of -270 mesh+400；
The preparation method of disperse carbon/carbon-copper composite material is：By Cu2O powder and Cu-Al-Y alloy powders are sufficiently mixed rear compressing
Billet, extrusion molding after the sintered internal oxidition processing of billet, forging, is produced；
Described to be compressed to the compacting of room temperature isostatic cool pressing, pressure is 270 ~ 380MPa, and pressing speed is 40 ~ 60MPa/min, during pressurize
Between be 2 ~ 10min；
The temperature of the sintering internal oxidition is 950 ~ 1000 DEG C, and soaking time is 2 ~ 10h；
The 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；
Described to be forged to cold closed-die forging deformation, deflection is 60 ~ 80%.
2. disperse carbon/carbon-copper composite material according to claim 1, it is characterised in that：By the component system of following mass percent
Into：Cu2O powder 1.58 ~ 18.96%, surplus are Cu-Al-Y alloy powders.
3. the preparation method of disperse carbon/carbon-copper composite material as claimed in claim 1 or 2, it is characterised in that：By Cu2O powder and Cu-
Al-Y alloy powders are sufficiently mixed rear compressing billet, extrusion molding after the sintered internal oxidition processing of billet, forging, i.e.,
；
Described to be compressed to the compacting of room temperature isostatic cool pressing, pressure is 270 ~ 380MPa, and pressing speed is 40 ~ 60MPa/min, during pressurize
Between be 2 ~ 10min；
The temperature of the sintering internal oxidition is 950 ~ 1000 DEG C, and soaking time is 2 ~ 10h；
The 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；
Described to be forged to cold closed-die forging deformation, deflection is 60 ~ 80%.
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| CN106191506B (en) * | 2016-07-12 | 2017-09-01 | 黄天增 | A kind of preparation technology of external oxidation dispersion strengthening copper alloy |
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| CN107863199B (en) * | 2017-10-11 | 2019-04-23 | 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 |
| 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 |
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