CN103451466A - Method for preparing high-smelting-point hard particle dispersion strengthened copper-base composite material by liquid-phase sintering and electromagnetic sintering device - Google Patents
Method for preparing high-smelting-point hard particle dispersion strengthened copper-base composite material by liquid-phase sintering and electromagnetic sintering device Download PDFInfo
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- CN103451466A CN103451466A CN2013100174009A CN201310017400A CN103451466A CN 103451466 A CN103451466 A CN 103451466A CN 2013100174009 A CN2013100174009 A CN 2013100174009A CN 201310017400 A CN201310017400 A CN 201310017400A CN 103451466 A CN103451466 A CN 103451466A
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Abstract
The invention discloses a method for preparing a high-smelting-point hard particle dispersion strengthened copper-base composite material by liquid-phase sintering. The method is composed of four main steps of preparing mixed powder, preparing a copper-base composite material pre-fabricated blank, carrying out liquid-phase sintering under a stable and constant magnetic field and cooling a dense high-strength copper-base composite material billet. The liquid-phase sintering is used for endowing the copper-base composite material with the highest strength and density; meanwhile, the constant magnetic field is used for improving the viscosity of a copper melt in the liquid-phase sintering; a magnetic field force and a Lorentz force are used for inhibiting the movement of high-smelting-point hard material particles in copper liquid and preventing clustering and layering of the high-smelting-point hard material particles so as to prepare a high-strength and high-conductivity copper alloy billet with excellent mechanical property and conductivity. The invention further provides a high-strength and high-conductivity copper alloy sintering device which comprises a heating and heat insulation device, an atmosphere control device and a stable and constant magnetic field generation device. According to the invention, the technical target of guaranteeing the high strength and the high conductivity of the copper-base composite material can be reached and a great industrial application value is realized.
Description
Technical field
The present invention relates to method for preparing powder metallurgy and the agglomerating plant of a kind of fabrication process of metal matrix composites and equipment, particularly a kind of Cu-base composites.
Background technology
Copper and alloy thereof are one of most important function and structure materials in the development of the national economy, and the electroconductibility that it is good and corrosion resistance nature can be widely used in the various fields such as communication, electric power, aerospace, traffic, household, automatization.Yet the electroconductibility of copper alloy and intensity are the character of conflict, often will take the electroconductibility of sacrificing copper alloy for the intensity that improves copper alloy is cost.As alloys such as the copper magnesium of current widespread use, copper tin, copper chromium, copper iron phosphorus, although its intensity is higher, but its specific conductivity often can only reach the 50-80% of fine copper specific conductivity, if use this structured material that has conducting function concurrently, often there is huge electric energy loss.Therefore, how to take into account intensity and the specific conductivity of copper alloy, become the bottleneck problem for preparing copper alloy with high strength and high conductivity.From the alloying angle, due to the specific conductivity of most alloying elements all significantly lower than the specific conductivity of copper, therefore the alloying element added for raising copper alloy intensity inevitably can significantly reduce the specific conductivity of copper alloy, therefore, for high conductivity and the intensity of guaranteeing copper alloy, precipitation strength mechanism based on Ao Luowan mechanism (Orowan) and toward the fine second-phase ceramic particle (aluminum oxide of interpolation in copper alloy, silicon carbide, titanium boride etc.) method, due to compound working hardening effect, obtaining the high-intensity while, can make more than the specific conductivity of copper alloy reaches 90%IACS, thereby can realize the high strength of copper alloy and the target that high conductivity is taken into account.
Be most widely used at present second phase particles precipitation strength copper alloy be the alumina dispersion-strenghtened copper alloy.Because the alumina dispersion-strenghtened copper alloy has good comprehensive physical mechanical property, there is higher specific tenacity, specific modulus, good electroconductibility, thermal conductivity, wear resistance, resistance to elevated temperatures, low thermal expansivity, the high over-all propertieies such as dimensional stability, its softening temperature can reach 930 ℃, specific conductivity can reach 54MS/m (92.4%IACS), more than tensile strength can reach 540MPa, therefore can be applied to the lead frame of unicircuit, various spot welding, the electrode of roll seam welding machine, contact material, the reverser of armature, the rotor line of large high-speed turbodynamo, the high conductivity that the aerial condutor of large electric locomotive etc. require, high-intensity components and parts etc.
For the aluminum oxide dispersion copper alloy, how fine alumina particle disperse is distributed in to the emphasis place that the copper matrix is this copper alloy with high strength and high conductivity of preparation.The method for preparing at present the alumina dispersion-strenghtened copper alloy mainly contains: stirring casting method, thermal reduction method of formation, Tai-Ace S 150 decomposition method, RAD method, internal oxidation, composite electroplating, machine-alloying and powder metallurgic method etc.Stirring casting method is to manufacture aluminum oxide dispersion copper alloy method the earliest, but due to Cu and Al
2o
3the wettability of particle is poor, how fine alumina particle disperse is distributed in copper melts, also will overcomes that the dispersion of alumina particle is inhomogeneous and to overcome that floating that huge density difference causes alumina particle reunites be the method insurmountable problem always simultaneously.The thermal reduction method of formation is to select Cu-Al powdered alloy, Cu
2the O powder is made powder compact, then pressed compact is entered in copper alloy in molten copper temperatures, and the particulate matter that reaction generates is distributed in Cu liquid under the effect of electromagnetic stirring force.Because Al is more much bigger than the avidity of Cu and O with the avidity of O, so Cu
2o can be very fast by the Al oxidation and itself is reduced.But this method is difficult to control the even diffusion of powder compact in copper liquid, the enhanced granule disperse that causes reaction to generate is inhomogeneous, affects the performance of material.The Tai-Ace S 150 decomposition method by adding pretreated Al in copper liquid
2(SO
4)
3powder, Al
2(SO
4)
3decomposes generates Al
2o
3thereby, preparation Cu-Al
2o
3matrix material, the shortcoming of this method is reactant A l
2(SO
4)
3thereby the little difficulty that adds of density, and the composite property made is unstable.The RAD method is with containing O in course of injection
2n
2carry out atmosphere protection, utilize N
2in O
2make Al preferential oxidation reaction generate Al
2o
3enhanced granule, the cooling rear formation Cu-Al of deposition in substrate
2o
3matrix material, this method apparatus expensive, complex process, be not suitable for suitability for industrialized production.Internal oxidation is that aluminium is joined in copper melts and forms X alloy, with high pressure nitrogen atomization melt, thereby make copper-aluminum alloy powder, powder is mixed to post-heating to high temperature mutually with oxygenant (thin cupric oxide powder), copper oxide decomposes, the oxygen simultaneously generated is diffused in copper aluminium solid solution alloy, and aluminum ratio copper easily generates oxide compound, and the aluminium in alloy is generated Al by preferential oxidation
2o
3, after whole aluminium is all oxidized, under hydrogen or cracked ammonium atmosphere, by the powder heating, remove the excess of oxygen in powder, finally make the copper powder of dispersion-strengthened.This kind of method prepared to the method compression moulding that the dispersion oxidation copper powder adopts hot isostatic pressing, or be rolled moulding, can obtain the copper alloy with high strength and high conductivity that dispersion oxidation aluminium strengthens.The weak point of the method is that operation is various, and cost is high, can't produce the alloy material of large-scale or long size.Composite electroplating is the novel method grown up over nearly 20 years, is co-deposited to cathode surface by the aluminum oxide by plating solution and matrix metal copper or alloy and forms composite deposite, thereby greatly improve the performance of material.Composite electroplating preparation technology is simple, but alumina particle even suspension in plating solution is wayward, can't make the aluminum oxide even dispersion in copper, and preparation cost is higher, can't scale operation.Mechanical alloying method adopts high energy ball mill to make Cu powder and Al
2o
3be uniformly distributed, but large than internal oxidation of grain-size makes composite powder by this method and there will be the segregation of wild phase and grow up in sintering process, thereby affect the performance of matrix material, in addition, the method not only preparation cost is high, and is difficult to equally prepare large-sized composite members.
Powder metallurgic method is a certain proportion of Cu powder and Al
2o
3the enhanced granule powder mixes, and carries out sintering after compression moulding, makes the sintered compact prefabricated component.Then by liquid infiltration to infiltration copper in the reinforcement prefabricated component.Powder metallurgic method is with respect to other method, technical maturity, and the quality and performance of material is very superior all.But adopt liquid infiltration infiltration copper means to increase the complicacy of production technique, in the infiltration process, if adopt the pressure infiltration can make prefabricated component pore be arranged with loose, the while is yielding and skew also; If adopt the vacuum-pressure infiltration method, be vulnerable to the limitation of equipment.Once the formation liquid phase, be difficult to suppress the gathering of liquid phase copper and the floating layering of aluminum oxide powder, thereby the performance of dispersion strengthening copper alloy reduced greatly.And do not adopt the method for liquid-phase infiltrating, the intensity of sintered compact is very low, and has a large amount of holes, can't improve its mechanical property.Therefore, if reunion and layering by aluminum oxide in certain technology controlling and process liquid phase sintering or infiltration process, just be expected to obtain the alumina dispersion-strenghtened copper alloy material of excellent performance, method and the electromagnetism agglomerating plant of developing practical Cu-base composites remain key issue urgently to be resolved hurrily.
Summary of the invention
In order to solve the prior art problem, the object of the invention is to overcome the defect that prior art exists, provide liquid phase sintering under a kind of steady magnetic field to prepare method and the electromagnetism agglomerating plant of high-melting-point hard material particle dispersed and strengthened copper-based composite material, utilize liquid phase sintering to make Cu-base composites obtain the highest intensity and density, utilize stationary magnetic field to strengthen the viscosity of copper melts in liquid phase sintering simultaneously, utilize magnetic field force and lorentz's force to suppress the motion of high-melting-point hard material particle in copper liquid, prevent reunion and the layering of high-melting-point hard material particle, thereby the copper alloy with high strength and high conductivity billet that the mechanical property of preparing and conductivity are more excellent, reach the high strength of Cu-base composites and the technical object that high conductivity is taken into account, realize huge industry using value.
Create purpose for reaching foregoing invention, design of the present invention is as follows:
Traditional powder metallurgic method prepares high-melting-point hard material particle dispersed and strengthened copper-based composite material, when making the sintered compact prefabricated component, is to obtain final copper base composite wood base by liquid infiltration to infiltration copper in reinforcement.The method complex process, the composite material interface vulnerable to pollution, and production process can't be stablized control.For addressing this problem, the present invention's imagination, prefabricated component for the high-melting-point hard material particle dispersed and strengthened copper-based composite material that adopts prior powder metallurgy method or internal oxidation to prepare, adopt the method for liquid phase sintering, improve its bonding properties, and in liquid sintering process, for the appearance of avoiding liquid phase copper causes reunion and the layering of high-melting-point hard material particle, apply a strong static magnetic field, the viscosity that the magnetic field force produced due to magnetic field and lorentz's force can significantly strengthen copper melts, suppress the motion of high-melting-point hard material particle in copper melts, therefore can significantly strengthen the resistance of motion of high-melting-point hard material particle, thereby can prevent its reunion and layering, again in conjunction with quick cooling mode, just can obtain the fine and close billet of the high-melting-point hard material particle dispersed and strengthened copper-based composite material of excellent performance.
According to above inventive concept, the present invention adopts following technical proposals:
Under a kind of steady magnetic field, liquid phase sintering prepares the method for high-melting-point hard material particle dispersed and strengthened copper-based composite material, comprises the steps:
A. the preparation of mixed powder: will be containing copper powder and high-melting-point hard material powder according to the full and uniform mix of preset blending ratio, obtain mixed powder, be respectively nanoscale powder, micron powder or different nano level and micron order granularity mixed powders containing copper powder and high-melting-point hard material powder, the fusing point of high-melting-point mechanically resistant material is higher than containing the fusing point of copper powder, and the high-melting-point mechanically resistant material under hot conditions not with containing various element generation chemical reactions in copper powder; The high-melting-point mechanically resistant material preferably adopts hard high-melting-point pottery or hard refractory metal; Containing copper powder, be fine copper powder or copper alloy powder; Hard high-melting-point pottery preferably adopts aluminum oxide, silicon carbide, titanium boride or zirconium white; The process of mix preferably adopts V-type mixer or planetary ball mill to carry out, and the batch mixing rotating speed is 10-1500r/min, and mixing time is 0.5-240h, and the batch mixing process is carried out under the protection of rare gas element or reducing gas; Perhaps the process of mix adopts internal oxidation to prepare mixed powder especially;
B. the preparation of Cu-base composites precast billet: to the mixed powder prepared, by press working or compression moulding mode, prepare the Cu-base composites precast billet in step a;
C. liquid phase sintering under steady magnetic field: in liquid sintering process, not with the non-oxide protective atmosphere condition of Cu-base composites precast billet chemical reaction under or under the vacuum protection condition, the Cu-base composites precast billet prepared in step b is carried out to liquid phase sintering, apply strong static magnetic field to the Cu-base composites precast billet simultaneously, make the Cu-base composites precast billet fully under steady magnetic field, the magnetic field force and the lorentz's force that utilize magnetic field to produce suppress the motion of high-melting-point hard material particle disperse in the conductive melt of cupric, increase the virtual viscosity of conductive melt, strengthen the resistance of motion of high-melting-point hard material particle, the high-melting-point hard material particle that makes to be suspended in conductive melt keeps original position, prevent reunion and the layering of high-melting-point hard material particle, thereby make high-melting-point hard material particle even dispersion in conductive melt, steady magnetic field is preferably the stationary magnetic field applied in whole liquid sintering process, perhaps adopt especially the timesharing stationary magnetic field of the different magnetic induction density of setting respectively in sintering intensification, cooling and insulating process, or adopt especially the piecewise constant magnetic field of monotone variation with the sintering temperature difference according to magnetic induction density, the stationary magnetic field that steady magnetic field is preferably produced by superconducting magnet, resistance magnet or superconduction-resistance hybrid magnet, its magnetic induction density is 0.01-20T, the room temperature bore of magnet is 50-1500mm, the magnetic line of force direction is preferably parallel or vertical with the axial direction due of Cu-base composites precast billet, non-oxide protective atmosphere is provided by rare gas element, reducing gas or the mixed gas that formed by rare gas element and reducing gas, rare gas element is preferably any one gas or any several mixed gas in nitrogen, argon gas and helium, and reducing gas is preferably any one gas or any several mixed gas in hydrogen, methane and carbon monoxide, sintering temperature preferably is controlled at 900 ~ 1300 ℃, and soaking time is preferably 0.5 ~ 240 hour, and temperature rise rate and rate of temperature fall are 0.1-1000 ℃/min,
D. compact high-strength degree Cu-base composites billet is cooling: the conductive melt of the even dispersion high-melting-point hard material particle for preparing in step c is carried out cooling fast, obtain the high-strength copper based composites billet of densification of the copper alloy of high-melting-point hard material particle dispersion-strengthened.
In order to realize that liquid phase sintering of the present invention prepares the method for high-melting-point hard material particle dispersed and strengthened copper-based composite material, a kind of electromagnetism agglomerating plant also is provided, by heating and heat-insulating device, atmosphere control device and steady magnetic field generating unit, formed, be specially:
Heating and heat-insulating device is by the stainless steel body of heater, crucible, refractory fibre, heating unit, temperature regulating device, thermopair, back-up block, heat insulation block and water cold sleeve form, load Cu-base composites precast billet to be sintered in crucible, the back-up block of installing in crucible bottom is arranged on heat insulation block, crucible is placed in to the refractory fibre cover central authorities that inside arranges the tubular of heating unit, refractory fibre, heat insulation block is positioned over furnace shell together with crucible the whole series, in the inner chamber of the cup-shaped stainless steel body of heater of water cold sleeve and atmosphere control device, the sealing bell that also is provided with suitable for reading of stainless steel body of heater, water cold sleeve is cooling to the sidewall of stainless steel body of heater, heating unit is connected with external power source integrated in temperature regulating device, detect in real time the temperature in the inner chamber of stainless steel body of heater by thermopair, temperature regulating device is formed to signal feedback, and and then control the heat energy output of heating unit, make melting containing copper powder particles in the Cu-base composites precast billet, form conductive melt, atmosphere control device comprises gas piping, rare gas element air intake valve and vacuum extraction valve, Sealing furnace covers and is provided with vacuum pumping port and the inert gas import formed by gas piping, and respectively by rare gas element air intake valve and vacuum extraction valve gate control rare gas element air inlet with carry out vacuum suction, the steady magnetic field generating unit is arranged at the cooling surface position of water cold sleeve around the stainless steel body of heater, in the steady strong static magnetic field that whole Cu-base composites precast billet is applied in the steady magnetic field generating unit fully, the magnetic field force and the lorentz's force that utilize magnetic field to produce suppress the motion of high-melting-point hard material particle disperse in the conductive melt of cupric, increase the virtual viscosity of conductive melt, strengthen the resistance of motion of high-melting-point hard material particle, the high-melting-point hard material particle that makes to be suspended in conductive melt keeps original position, prevent reunion and the layering of high-melting-point hard material particle, thereby make high-melting-point hard material particle even dispersion and hover in conductive melt.
The direction of the magnetic line of force of the steady strong static magnetic field that above-mentioned steady magnetic field generating unit applies be preferably vertically to or horizontal direction.
The present invention compared with prior art, has following apparent outstanding substantive distinguishing features and remarkable advantage:
1. adopt powder metallurgic method to prepare high-melting-point hard material particle dispersed and strengthened copper-based composite material, can control exactly the consumption of Cu-base composites and high-melting-point mechanically resistant material, thereby obtain containing copper mass or mechanically resistant material massfraction difference, performance is different Cu-base composites also.
2. adopt the method for liquid phase sintering, avoided the prior powder metallurgy method in the process of infiltration copper, the limitation of the distortion of prefabricated component and skew and equipment.
3. the steady magnetic field added can be in the 0.01-20T range, by magnetic field, second phase particles motion in conductive melt there is the effect of a very strong inhibition, can increase the virtual viscosity of liquid phase copper liquid simultaneously, thereby make high-melting-point hard material particle energy even dispersion in copper liquid, make the high-melting-point hard material particle dispersed and strengthened copper-based composite material that over-all properties is superior.
4. the steady magnetic field adopted is a kind of physical field of cleaning, and environment is not polluted, and material is not polluted yet simultaneously, and the Cu-base composites purity made is higher.
5. present method adopts cryogenic magnetic field, because the superconducting state coil does not have resistance, therefore without consumed energy, only need provide the refrigerator that maintains superconducting temperature less electric power, and the room temperature bore maximum of superconducting magnet can reach 300-2000mm at present, can be satisfied with the liquid phase sintering of the sample of large-size fully, therefore adopt present method, with low cost, technique is simple, is expected to carry out large-scale industrial production.
The accompanying drawing explanation
Fig. 1 is the embodiment of the present invention one electromagnetism agglomerating plant structural representation.
Embodiment
Details are as follows for the preferred embodiments of the present invention:
embodiment mono-:
The present embodiment adopts the high-melting-point mechanically resistant material of alumina powder as dispersion-strengthened, adopts the copper alloy preparation containing copper powder, makes Cu-Al
2o
3powder circle base precast billet is carried out powder metallurgy, prepares the high-strength copper based composites billet of densification of the copper alloy of high-melting-point hard material particle dispersion-strengthened.
In the present embodiment, referring to Fig. 1, for realizing that liquid phase sintering prepares the electromagnetism agglomerating plant of the method for high-melting-point hard material particle dispersed and strengthened copper-based composite material, by heating and heat-insulating device, atmosphere control device and steady magnetic field generating unit 10, formed, be specially:
Heating and heat-insulating device is by stainless steel body of heater 11, crucible 5, refractory fibre 6, heating unit 4, temperature regulating device 1, thermopair 3, back-up block 7, heat insulation block 8 and water cold sleeve 9 form, the Cu-base composites precast billet 14 that the interior loading of crucible 5 is to be sintered, the back-up block 7 of installing in crucible 5 bottoms is arranged on heat insulation block 8, crucible 5 is placed in to the refractory fibre 6 cover central authorities that inside arranges the tubular of heating unit 4, refractory fibre 6, heat insulation block 8 is positioned over furnace shell together with crucible 5 the whole series, in the inner chamber of the cup-shaped stainless steel body of heater 11 of water cold sleeve 9 and atmosphere control device, the sealing bell that also is provided with suitable for reading of stainless steel body of heater 11, the sidewall of 9 pairs of stainless steel bodies of heater 11 of water cold sleeve is cooling, heating unit 4 is connected with external power source integrated in temperature regulating device 1, by the temperature in the inner chamber of the real-time detection stainless steel of thermopair 3 body of heater 11, temperature regulating device 1 is formed to signal feedback, and and then control the heat energy output of heating unit 4, make melting containing copper powder particles 16 in Cu-base composites precast billet 14, form conductive melt 18, atmosphere control device comprises gas piping 2, rare gas element air intake valve 12 and vacuum extraction valve 13, Sealing furnace covers and is provided with vacuum pumping port and the inert gas import formed by gas piping 2, and controls the rare gas element air inlet and carry out vacuum suction by rare gas element air intake valve 12 and vacuum extraction valve 13 respectively, steady magnetic field generating unit 10 is arranged at the cooling surface position of water cold sleeve 9 around stainless steel body of heater 11, in the steady strong static magnetic field that whole Cu-base composites precast billet 14 is applied in steady magnetic field generating unit 10 fully, the magnetic field force and the lorentz's force that utilize magnetic field to produce suppress the motion of high-melting-point hard material particle 17 disperses in the conductive melt 18 of cupric, increase the virtual viscosity of conductive melt 18, strengthen the resistance of motion of high-melting-point hard material particle 17, the high-melting-point hard material particle 17 that makes to be suspended in conductive melt 18 keeps original position, prevent reunion and the layering of high-melting-point hard material particle 17, thereby make high-melting-point hard material particle 17 even dispersion and hover in conductive melt 18.
Adopt the Cu-Al that the Cu massfraction is 99.8%
2o
3alloy, prepare the embodiment alloy of the method and apparatus of alumina dispersion-strenghtened copper alloy as liquid phase sintering under steady magnetic field.Take Micron-Sized Copper Powders Coated 19600g and nano level pure zirconia aluminium powder 40g, the average particle diameter of nano aluminium oxide is 30 nanometers, puts it in the V-type mixer and mixes; it is mixed; batch mixing speed is 50r/min, and mixing time is 8h, logical argon shield in mixer in the batch mixing process.After finishing, batch mixing takes out the Cu-Al mixed
2o
3powder, the Cu-Al that pressure rolling Cheng Gaowei 300mm, diameter are 300mm
2o
3powder circle base, square billet or slab.
In the present embodiment, under steady magnetic field, liquid phase sintering prepares the alumina dispersion-strenghtened copper alloy, and its sintering process is realized by atmosphere under steady magnetic field or vacuum protection liquid phase sintering device.Referring to Fig. 1, implement when of the present invention, by the Cu-Al of above-mentioned preparation
2o
3powder compact is put in the crucible 5 of the corundum in stainless steel body of heater 11, and crucible 5 use back-up blocks 7 and heat insulation block 8 support fixing.Open vacuum extraction valve 13, adopt mechanical pump and diffusion pump to be pumped into 10 in stainless steel body of heater 11
-3pa, close vacuum extraction valve 13, opens rare gas element air intake valve 12, in stainless steel body of heater 11, is filled with high-purity argon gas to 0.8atm, then closes rare gas element air intake valve 12.The room temperature bore of magnet is 50mm-1500mm, opens steady magnetic field generating unit 10, makes magnetic induction density wherein reach 10 teslas, and the direction that guarantees magnetic line of force 15 for vertically to.Give in water-cooled sleeve pipe 9 and pass into water coolant, open temperature regulating device 1, by heating unit 4 and refractory fibre 6, the temperature in stainless steel body of heater 11 is heated to 1200 ℃ with the speed of 10 ℃/min, by thermopair 3, carry out monitor temperature.When temperature arrives 1200 ℃, be incubated 5 hours, now Cu-Al
2o
3copper powder particle 16 in pressed compact will be fused into the conductive melt 18 of liquid phase copper, motion inhibition due to 15 pairs of nano alumina particles of magnetic line of force, and the viscosity that increases liquid phase copper, therefore, nano alumina particles will keep original position, and copper powder particle 16 on every side will be due to liquid phase sintering by whole Cu-Al
2o
3pressed compact is connected to integral body.Then by temperature regulating device 1, make temperature in stainless steel body of heater 11 be cooled to room temperature with the speed of cooling of 100 ℃/min, then close temperature regulating device 1 and steady magnetic field generating unit 10, take out the Cu-Al sintered from stainless steel body of heater 11
2o
3pressed compact, can obtain the alloy billet of nano aluminium oxide even dispersion in copper.Then adopt conventional rolling, drawing process can prepare various alumina dispersion-strenghtened copper alloy bar materials, tubing, sheet material or silk material, and its intensity, conductivity excellence.
The concrete powder metallurgy process of the present embodiment is by mixed C u-Al
2o
3powder or interior cupric oxide powder, pressure rolling become liquid phase sintering Cu-Al under precast billet and steady magnetic field
2o
3three steps of pressed compact form.Pressed compact is adopted to the method for liquid phase sintering, add steady magnetic field in liquid sintering process, utilize magnetic field to Al simultaneously
2o
3the impact of disperse Homogenization Process in Cu liquid can be prepared the matrix material of the ODS copper-base alloys of excellent performance under simple processing condition.
embodiment bis-:
The present embodiment and embodiment mono-are basic identical, and special feature is:
In the present embodiment, change by preparing copper powder and micrometer alumina powder in above-described embodiment one copper powder that nano aluminum oxide dispersion prepared by internal oxidation distributes into, without mixed powder, direct pressing becomes pressed compact, then adopt with above-described embodiment one in same liquid sintering process, magnetic induction control is 16T, the liquid phase sintering temperature is 1100 ℃, be incubated 10 hours, can prepare equally the copper alloy with high strength and high conductivity billet of nano aluminum oxide dispersion strengthening.Then adopt conventional rolling, drawing process can prepare various nano aluminum oxide dispersion strengthened copper alloy bars, tubing, sheet material or silk material, and its intensity, conductivity excellence.
The above is illustrated the embodiment of the present invention by reference to the accompanying drawings, but the invention is not restricted to above-described embodiment, can also make multiple variation according to the purpose of innovation and creation of the present invention, the change of making under all spirit according to technical solution of the present invention and principle, modify, substitute, combination, simplify, all should be equivalent substitute mode, as long as goal of the invention according to the invention, only otherwise deviating from liquid phase sintering of the present invention prepares the method for high-melting-point hard material particle dispersed and strengthened copper-based composite material and know-why and the inventive concept of electromagnetism agglomerating plant, all belong to protection scope of the present invention.
Claims (10)
1. a liquid phase sintering prepares the method for high-melting-point hard material particle dispersed and strengthened copper-based composite material, it is characterized in that, comprises the steps:
A. the preparation of mixed powder: will be containing copper powder and high-melting-point hard material powder according to the full and uniform mix of preset blending ratio, obtain mixed powder, be respectively nanoscale powder, micron powder or different nano level and micron order granularity mixed powders containing copper powder and high-melting-point hard material powder, the fusing point of high-melting-point mechanically resistant material is higher than containing the fusing point of copper powder, and the high-melting-point mechanically resistant material under hot conditions not with containing various element generation chemical reactions in copper powder;
B. the preparation of Cu-base composites precast billet: to the mixed powder prepared, by press working or compression moulding mode, prepare the Cu-base composites precast billet in described step a;
C. liquid phase sintering under steady magnetic field: in liquid sintering process, not with the non-oxide protective atmosphere condition of Cu-base composites precast billet chemical reaction under or under the vacuum protection condition, the Cu-base composites precast billet prepared in described step b is carried out to liquid phase sintering, apply strong static magnetic field to the Cu-base composites precast billet simultaneously, make the Cu-base composites precast billet fully under steady magnetic field, the magnetic field force and the lorentz's force that utilize magnetic field to produce suppress the motion of high-melting-point hard material particle disperse in the conductive melt of cupric, increase the virtual viscosity of conductive melt, strengthen the resistance of motion of high-melting-point hard material particle, the high-melting-point hard material particle that makes to be suspended in conductive melt keeps original position, prevent reunion and the layering of high-melting-point hard material particle, thereby make high-melting-point hard material particle even dispersion in conductive melt,
D. compact high-strength degree Cu-base composites billet is cooling: the conductive melt of the even dispersion high-melting-point hard material particle for preparing in described step c is carried out cooling fast, obtain the high-strength copper based composites billet of densification of the copper alloy of high-melting-point hard material particle dispersion-strengthened.
2. liquid phase sintering according to claim 1 prepares the method for high-melting-point hard material particle dispersed and strengthened copper-based composite material, it is characterized in that: in described step a, the high-melting-point mechanically resistant material is hard high-melting-point pottery or hard refractory metal, and described is fine copper powder or copper alloy powder containing copper powder.
3. liquid phase sintering according to claim 2 prepares the method for high-melting-point hard material particle dispersed and strengthened copper-based composite material, it is characterized in that: hard high-melting-point pottery is aluminum oxide, silicon carbide, titanium boride or zirconium white.
4. according to any one in claim 1～3, described liquid phase sintering prepares the method for high-melting-point hard material particle dispersed and strengthened copper-based composite material, it is characterized in that: in described step c, the stationary magnetic field of steady magnetic field for applying in whole liquid sintering process, be perhaps the timesharing stationary magnetic field of the different magnetic induction density set respectively in sintering intensification, cooling and insulating process, or be the piecewise constant magnetic field of magnetic induction density with sintering temperature difference monotone variation.
5. according to any one in claim 1～3, described liquid phase sintering prepares the method for high-melting-point hard material particle dispersed and strengthened copper-based composite material, it is characterized in that: in described step c, steady magnetic field is the stationary magnetic field produced by superconducting magnet, resistance magnet or superconduction-resistance hybrid magnet, its magnetic induction density is 0.01-20T, and the room temperature bore of magnet is 50-1500mm; The magnetic line of force direction is parallel or vertical with the axial direction due of Cu-base composites precast billet.
6. according to any one in claim 1～3, described liquid phase sintering prepares the method for high-melting-point hard material particle dispersed and strengthened copper-based composite material; it is characterized in that: in described step c; non-oxide protective atmosphere is provided by rare gas element, reducing gas or the mixed gas that formed by rare gas element and reducing gas; rare gas element is any one gas or any several mixed gas in nitrogen, argon gas and helium, and reducing gas is any one gas or any several mixed gas in hydrogen, methane and carbon monoxide.
7. according to any one in claim 1～3, described liquid phase sintering prepares the method for high-melting-point hard material particle dispersed and strengthened copper-based composite material, it is characterized in that: in described step c, sintering temperature is 900 ~ 1300 ℃, soaking time is 0.5 ~ 240 hour, and temperature rise rate and rate of temperature fall are 0.1-1000 ℃/min.
8. according to any one in claim 1～3, described liquid phase sintering prepares the method for high-melting-point hard material particle dispersed and strengthened copper-based composite material, it is characterized in that: in described step a, the process of mix adopts V-type mixer or planetary ball mill to carry out, the batch mixing rotating speed is 10-1500r/min, mixing time is 0.5-240h, and the batch mixing process is carried out under the protection of rare gas element or reducing gas; Perhaps the process of mix adopts internal oxidation to prepare mixed powder.
9. realize that the described liquid phase sintering of any one in claim 1～3 prepares the electromagnetism agglomerating plant of the method for high-melting-point hard material particle dispersed and strengthened copper-based composite material for one kind, formed by heating and heat-insulating device, atmosphere control device and steady magnetic field generating unit (10), be specially:
Described heating and heat-insulating device is by stainless steel body of heater (11), crucible (5), refractory fibre (6), heating unit (4), temperature regulating device (1), thermopair (3), back-up block (7), heat insulation block (8) and water cold sleeve (9) form, load Cu-base composites precast billet (14) to be sintered in described crucible (5), the back-up block (7) of installing in described crucible (5) bottom is arranged on heat insulation block (8), described crucible (5) is placed in to described refractory fibre (6) the cover central authorities that inside arranges the tubular of heating unit (4), described refractory fibre (6), described heat insulation block (8) is positioned over furnace shell together with described crucible (5) the whole series, in the inner chamber of the cup-shaped described stainless steel body of heater (11) of water cold sleeve (9) and atmosphere control device, the sealing bell that also is provided with suitable for reading of described stainless steel body of heater (11), described water cold sleeve (9) is cooling to the sidewall of described stainless steel body of heater (11), described heating unit (4) is connected with external power source integrated in described temperature regulating device (1), detect in real time the temperature in the inner chamber of described stainless steel body of heater (11) by described thermopair (3), described temperature regulating device (1) is formed to signal feedback, and and then control the heat energy output of described heating unit (4), make melting containing copper powder particles (16) in Cu-base composites precast billet (14), form conductive melt (18),
Described atmosphere control device comprises gas piping (2), rare gas element air intake valve (12) and vacuum extraction valve (13), described Sealing furnace covers and is provided with vacuum pumping port and the inert gas import formed by described gas piping (2), and controls the rare gas element air inlet and carry out vacuum suction by described rare gas element air intake valve (12) and described vacuum extraction valve (13) respectively;
Described steady magnetic field generating unit (10) is arranged at the cooling surface position of described water cold sleeve (9) around described stainless steel body of heater (11), in the steady strong static magnetic field that whole Cu-base composites precast billet (14) is applied in described steady magnetic field generating unit (10) fully, the magnetic field force and the lorentz's force that utilize magnetic field to produce suppress the motion of high-melting-point hard material particle (17) disperse in the conductive melt (18) of cupric, increase the virtual viscosity of conductive melt (18), strengthen the resistance of motion of high-melting-point hard material particle (17), the high-melting-point hard material particle (17) that makes to be suspended in conductive melt (18) keeps original position, prevent reunion and the layering of high-melting-point hard material particle (17), thereby make high-melting-point hard material particle (17) even dispersion and hover in conductive melt (18).
10. electromagnetism agglomerating plant according to claim 9 is characterized in that: the direction of the magnetic line of force (15) of the steady strong static magnetic field that described steady magnetic field generating unit (10) applies for vertically to or horizontal direction.
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