CN112267041B - Composite bar and preparation method and application thereof - Google Patents
Composite bar and preparation method and application thereof Download PDFInfo
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- CN112267041B CN112267041B CN202011153134.9A CN202011153134A CN112267041B CN 112267041 B CN112267041 B CN 112267041B CN 202011153134 A CN202011153134 A CN 202011153134A CN 112267041 B CN112267041 B CN 112267041B
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- C22C1/00—Making non-ferrous alloys
- C22C1/04—Making non-ferrous alloys by powder metallurgy
- C22C1/05—Mixtures of metal powder with non-metallic powder
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- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
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- C22C1/00—Making non-ferrous alloys
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- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
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- C22F1/00—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
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- C22F—CHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
- C22F1/00—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
- C22F1/08—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working of copper or alloys based thereon
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Abstract
The invention relates to the technical field of copper alloy powder metallurgy and nonferrous metal processing, in particular to a composite bar and a preparation method and application thereof. The invention provides a preparation method of a composite bar, which comprises the following steps: mixing copper-aluminum alloy powder and cuprous oxide to obtain a mixture; fixing an oxygen-free copper bar at the center of a cold isostatic pressing die, uniformly filling the mixture around the oxygen-free copper bar, and carrying out cold isostatic pressing to obtain a cold isostatic pressing composite blank; sequentially carrying out heat treatment, hot extrusion compounding and drawing straightening on the cold isostatic pressing composite blank to obtain a composite bar; the heat treatment comprises internal oxidation, reduction and sintering; the composite bar comprises a core and a skin; the core part is made of oxygen-free copper; the outer skin is made of aluminum oxide dispersion strengthened copper alloy. The composite bar prepared by the invention has the characteristics of high strength, high conductivity, high temperature softening resistance and the like and good brazing performance.
Description
Technical Field
The invention relates to the technical field of copper alloy powder metallurgy and nonferrous metal processing, in particular to a composite bar and a preparation method and application thereof.
Background
The dispersion strengthening copper alloy is a copper alloy material formed by uniformly and dispersedly distributing ceramic particles with high melting point, high hardness, good thermal stability and chemical stability in a copper matrix. Compared with other strengthening modes, the dispersion strengthened mass points do not dissolve and grow up at high temperature, have strong barrier effect on dislocation movement and grain boundary migration, remarkably improve the strength and the high-temperature softening resistance of the material, and have small influence on free electron scattering, so that the conductivity of the copper matrix cannot be obviously reduced. The dispersion strengthened copper alloy has wide application, and relates to almost all fields of electronics, machinery, manufacturing, engineering application, aerospace and the like. However, the dispersion strengthened copper alloy has poor brazing performance, is a typical anti-adhesion material, and has unstable welding effect with oxygen-free copper, stainless steel and rare metal. Because the dispersion strengthened copper alloy has low density, the brazing filler metal is often absorbed by the dispersion strengthened copper alloy matrix, so that the brazing filler metal on the welding surface is lost, the welding strength is low, and even the phenomenon that a welding part directly falls off occurs.
The oxygen-free copper material has high purity, excellent electrical conductivity, thermal conductivity, cold and hot processability and good welding performance, has no hydrogen defect or few hydrogen defects, and is widely applied to parts such as busbars, conductive strips, waveguides, coaxial cables, vacuum sealing parts, vacuum tubes, transistors and the like. The oxygen-free copper can be brazed with other materials such as oxygen-free copper, stainless steel, ceramics, rare metals and the like in vacuum or hydrogen atmosphere, and the welding effect is good. However, after the oxygen-free copper is welded at 800-900 ℃, the material is obviously softened, and the application of the oxygen-free copper material is severely limited.
Therefore, how to combine the excellent characteristics of the aluminum oxide dispersion strengthened copper alloy and the oxygen-free copper alloy, develop the application potential of the two materials, fully exert the high-strength high-conductivity high-temperature softening resistance of the aluminum oxide dispersion strengthened copper alloy and the excellent brazing performance of the oxygen-free copper, and develop a composite plate with integrated functional structure is the object of research by people. At present, Chinese patent application No. 201711270364.1 discloses a powder metallurgy method for preparing a composite bar of dispersion strengthened copper alloy, which is suitable for brazing on the outer layer and is useless for workpieces needing brazing on the core.
Disclosure of Invention
The invention aims to provide a composite bar and a preparation method and application thereof.
In order to achieve the above object, the present invention provides the following technical solutions:
the invention provides a preparation method of a composite bar, which comprises the following steps:
mixing copper-aluminum alloy powder and cuprous oxide to obtain a mixture;
fixing an oxygen-free copper bar at the center of a cold isostatic pressing die, uniformly filling the mixture around the oxygen-free copper bar, and carrying out cold isostatic pressing to obtain a cold isostatic pressing composite blank;
sequentially carrying out heat treatment, hot extrusion compounding and drawing straightening on the cold isostatic pressing composite blank to obtain a composite bar;
the heat treatment comprises internal oxidation, reduction and sintering which are sequentially carried out;
the composite bar comprises a core and a skin;
the core part is made of oxygen-free copper;
the outer skin is made of aluminum oxide dispersion strengthened copper alloy.
Preferably, the preparation method of the copper-aluminum alloy powder is a water atomization method or a nitrogen atomization method;
the mass percentage of aluminum in the copper-aluminum alloy powder is 0.1-1.2%;
the granularity of the copper-aluminum alloy powder is-100 meshes.
Preferably, the pressure of the cold isostatic pressing is 180-240 MPa, the pressure maintaining time is 5-30 min, and three-stage pressure relief is adopted for pressure relief.
Preferably, the internal oxidation is carried out in an argon atmosphere, the temperature is 850-900 ℃, and the heat preservation time is 2-4 h;
the reduction is carried out in a hydrogen atmosphere, the temperature is 820-880 ℃, and the heat preservation time is 4-8 h;
the sintering is carried out in a hydrogen atmosphere, the temperature is 900-980 ℃, and the heat preservation time is 2-4 h.
Preferably, the temperature of hot extrusion compounding is 900-960 ℃, the heat preservation time is 1-3 h, and the extrusion ratio is 10-30 mm;
the diameter of the extrusion rod obtained after hot extrusion compounding is 13-25 mm.
Preferably, the mass percentage of the alumina in the alumina dispersion strengthened copper alloy is 0.2-2.4%.
Preferably, the diameter ratio of the core to the composite rod is (3-9): (8-20);
and the diameter of the composite rod is greater than the diameter of the core.
Preferably, the oxygen-free copper is under the brand name TU0, TU1 or TU 2.
The invention provides a preparation method of a composite bar, which comprises the following steps: mixing copper-aluminum alloy powder and cuprous oxide to obtain a mixture; fixing an oxygen-free copper bar at the center of a cold isostatic pressing die, uniformly filling the mixture around the oxygen-free copper bar, and carrying out cold isostatic pressing to obtain a cold isostatic pressing composite blank; sequentially carrying out heat treatment, hot extrusion compounding and drawing straightening on the cold isostatic pressing composite blank to obtain a composite bar; the heat treatment comprises internal oxidation, reduction and sintering; the composite bar comprises a core and a skin; the core part is made of oxygen-free copper; the outer skin is made of aluminum oxide dispersion strengthened copper alloy. The preparation method obtains the composite bar through heat treatment and hot extrusion, can be realized on the existing powder metallurgy production line, is easy to realize large-scale production, and has high production efficiency; in the manufacturing process of the high-performance welding, welding and cutting vulnerable parts, the phenomena of insufficient solder, desoldering and the like are easy to occur in the aluminum oxide dispersion strengthened copper alloy, the oxygen-free copper welding performance is excellent, but the post-welding strength is too low to clamp and seal. By embedding the oxygen-free copper into the aluminum oxide dispersion strengthened copper alloy bar core part, the excellent welding performance of the oxygen-free copper is utilized to ensure full and firm welding, and meanwhile, the outer aluminum oxide dispersion strengthened copper alloy layer keeps better strength to meet the requirements of clamping and sealing. Therefore, the composite bar prepared by the invention organically combines the excellent characteristics of high strength, high conductivity, high temperature softening resistance and the like of the aluminum oxide dispersion strengthened copper alloy and the excellent brazing performance of oxygen-free copper, and has complementary advantages, so that the composite bar has the excellent characteristics of high strength, high conductivity, high temperature softening resistance and the like and the excellent brazing performance.
Drawings
FIG. 1 is a schematic longitudinal sectional view of the composite bar according to the present invention;
FIG. 2 is an interfacial metallographic image of a composite rod prepared in example 1.
Detailed Description
The invention provides a preparation method of a composite bar, which comprises the following steps:
mixing copper-aluminum alloy powder and cuprous oxide to obtain a mixture;
fixing an oxygen-free copper bar at the center of a cold isostatic pressing die, uniformly filling the mixture around the oxygen-free copper bar, and carrying out cold isostatic pressing to obtain a cold isostatic pressing composite blank;
sequentially carrying out heat treatment, hot extrusion compounding and drawing straightening on the cold isostatic pressing composite blank to obtain a composite bar;
the heat treatment comprises internal oxidation, reduction and sintering which are sequentially carried out;
the composite bar comprises a core and a skin;
the core part is made of oxygen-free copper;
the material of the outer skin is aluminum oxide dispersion strengthened copper alloy (the longitudinal section structure is shown in figure 1).
In the present invention, all raw materials are commercially available products of resins to those skilled in the art, if specifically noted.
In the present invention, the oxygen-free copper is preferably of the brand TU0, TU1 or TU 2.
In the invention, the mass percentage content of the aluminum oxide in the aluminum oxide dispersion strengthened copper alloy is preferably 0.2-2.4%, more preferably 0.5-2.0%, and most preferably 1.0-1.5%.
In the invention, the diameter ratio of the core to the composite bar is preferably (3-9): (8-20), more preferably (5-8): (12-18). In a specific embodiment of the invention, the diameter of the core is preferably 3-9 mm, more preferably 8-20 mm, and the diameter of the composite rod is preferably 8-20 mm, more preferably 12-18 mm.
In the invention, the interface between the oxygen-free copper and the aluminum oxide dispersion strengthened copper alloy has no delamination, no bubble and no inclusion.
The invention mixes copper aluminum alloy powder and cuprous oxide to obtain a mixture. In the invention, the copper-aluminum alloy powder is preferably prepared, and the preparation method of the copper-aluminum alloy powder is preferably a water atomization method or a nitrogen atomization method; the specific process of the water atomization method or the nitrogen atomization method is not limited in any way, and the process known to those skilled in the art can be adopted.
In the invention, the mass percentage of aluminum in the copper-aluminum alloy powder is preferably 0.1-1.25%, and more preferably 0.5-1.0%. In the invention, the granularity of the copper-aluminum alloy powder is preferably-100 meshes. In the present invention, the source of cuprous oxide is preferably commercial cuprous oxide or self-made cuprous oxide.
In the invention, the mass ratio of the copper-aluminum alloy powder to the cuprous oxide is Al generated by the reaction of Al and O2O3The above-mentioned components are mixed in a ratio of 0.8 to 1.3, and the excess coefficient of O is preferably set to 0.8 to 1.3. In the present invention, the mixing is preferably carried out in a mixer, preferably a double cone mixer or a ballAnd (5) grinding. The rotating speed of the mixer is not limited in any way, and can be realized by adopting a rotating speed well known by the technical personnel in the field.
After the mixture is obtained, the oxygen-free copper rod is fixed in the center of a cold isostatic pressing die, the mixture is uniformly filled around the oxygen-free copper rod, and cold isostatic pressing is carried out to obtain the cold isostatic pressing composite blank.
In the invention, the diameter of the oxygen-free copper rod is preferably 25-40 mm.
In the present invention, before the cold isostatic pressing, in order to prevent the pressurized medium liquid from penetrating into the powder, it is preferable to fix an oxygen-free copper rod in the center of the cold isostatic pressing mold, fill the mixture uniformly around the oxygen-free copper rod, plug the mold with a rubber plug, and tie and seal with a metal wire.
In the invention, the pressure of the cold isostatic pressing is preferably 180-240 MPa, and more preferably 200-220 MPa; the pressure maintaining time is preferably 5-30 min, more preferably 10-25 min, and most preferably 15-20 min; after the cold isostatic pressing is finished, the invention preferably adopts a three-level pressure relief mode for pressure relief; the process of the three-stage pressure relief is not limited in any way, and can be performed by a process well known to those skilled in the art.
After the cold isostatic pressing composite blank is obtained, the cold isostatic pressing composite blank is sequentially subjected to heat treatment, hot extrusion compounding and drawing straightening to obtain the composite bar.
In the present invention, the heat treatment includes internal oxidation, reduction and sintering in this order; the internal oxidation is preferably carried out in an argon atmosphere, the temperature of the internal oxidation is preferably 850-900 ℃, more preferably 860-880 ℃, and the heat preservation time is preferably 2-4 hours, more preferably 2.5-3.5 hours; the reduction is preferably carried out in a hydrogen atmosphere, and the temperature of the reduction is preferably 820-880 ℃, more preferably 840-860 ℃; the heat preservation time is preferably 4-8 h, and more preferably 6-7 h; the sintering is preferably carried out in a hydrogen atmosphere, the temperature is preferably 900-980 ℃, and more preferably 920-960 ℃; the heat preservation time is preferably 2-4 h, and more preferably 2.5-3.5 h.
In the present invention, the internal oxidation occurs [ Al]The preferential oxidation of the aluminum oxide particles has the function of producing dispersion strengthening particle nano aluminum oxide particles; the reduction takes place by a hydrogen reduction reaction which acts to reduce the residual [ O ] remaining after the internal oxidation process]By H2Reducing to reduce the oxygen content in the material; the sintering is solid phase sintering, and the function is to accelerate the diffusion process through the temperature effect and enable partial metallurgical bonding to be generated among powder particles.
In the invention, the temperature of hot extrusion compounding is preferably 900-960 ℃, and more preferably 920-940 ℃; the heat preservation time is preferably 1-3 h, and more preferably 1.5-2.5 h; the extrusion ratio is preferably 10-30 mm, and more preferably 15-25 mm; the diameter of the extrusion rod obtained after hot extrusion compounding is preferably 13-25 mm, and more preferably 15-20 mm.
In the present invention, before the straightening, the head and the tail of the pressed bar are preferably removed and the scale is preferably removed. The removal method is not limited in any way, and can be removed by a method known to those skilled in the art. In the invention, the drawing straightening comprises drawing and straightening; in the present invention, the drawing is preferably performed by cold drawing on a chain type drawing machine. The cold drawing process on the chain type drawing machine is not limited in any way, and the cold drawing process can be carried out by adopting a process well known to a person skilled in the art.
After the drawing, the obtained composite bar is preferably sawed and straightened by the method; the sawing and straightening process is not subject to any particular restrictions by the present invention, and can be carried out using processes known to those skilled in the art.
The following examples are provided to illustrate the composite rods of the present invention and the method and application thereof in detail, but they should not be construed as limiting the scope of the present invention.
Example 1
Water atomized Cu-Al alloy powder (Al content 0.1 wt%) with granularity of-100 mesh and commercial cuprous oxide are reacted with O to generate Al2O3The excess coefficient of O is 0.8, mixing for 4 hours in a double-cone mixer to obtain a mixture;
an oxygen-free copper rod with the diameter of 25mm and the brand number of TU2 is fixed in the center of a mould for cold isostatic pressing, then the mixture is uniformly filled around the oxygen-free copper rod, a rubber plug is used for plugging the mould, and a metal wire is used for tightly fastening and sealing to prevent the pressurized medium liquid from permeating into the powder. Placing the assembled die in a cold isostatic press for compression molding, wherein the pressure of the cold isostatic press is 200MPa, the pressure maintaining time is 8min, and the pressure is relieved by adopting three-stage pressure relief to obtain a cold isostatic press composite blank;
sequentially carrying out internal oxidation (argon atmosphere, 850 ℃,2h), reduction (hydrogen atmosphere, 820 ℃,4h) and sintering (hydrogen atmosphere, 900 ℃,4h) on the cold isostatic pressing composite blank, carrying out hot extrusion compounding (temperature is 900 ℃, heat preservation time is 1h, extrusion ratio is 22, diameter of the obtained extrusion rod is 17mm), removing head, tail and oxide skin from the hot extrusion compounded composite blank, carrying out cold drawing treatment on a chain type drawing machine, and finally carrying out saw cutting and straightening to obtain a composite bar with diameter of 13 mm;
wherein, FIG. 2 is the interface gold phase diagram of the composite bar, and as can be seen from FIG. 2, the interface between the oxygen-free copper and the aluminum oxide dispersion strengthened copper alloy has no delamination, no bubble and no inclusion;
the diameter of the composite bar is 13mm, the diameter of the core part is 6mm, and Al in the aluminum oxide dispersion strengthened copper alloy2O3The mass percentage content of the compound is 0.2 percent;
and (3) performing hardness test on the composite bar according to GB/T230.1-2004 standard, and performing conductivity test on the composite bar according to YS/T478-2005 standard, wherein the test results show that the hardness of the oxygen-free copper is 62HRB, the hardness of the outer edge aluminum oxide dispersion strengthened copper alloy is 72HRB, and the overall conductivity is 95.7% IACS.
Example 2
Water atomized Cu-Al alloy powder (Al content 1.2 wt%) with granularity of-100 mesh and commercial cuprous oxide are reacted with O to generate Al2O3According to the ratio of (1) and the excess coefficient of O of 1.3 for 10hThe preparation method comprises the following steps of (1) performing in a double-cone mixer to obtain a mixture;
fixing an oxygen-free copper rod with the diameter of 40mm and the brand number of TU0 in the center of a mould for cold isostatic pressing, then uniformly filling the mixture around the oxygen-free copper rod, plugging the mould with a rubber plug, and tightly sealing with a metal wire to prevent the pressurized medium liquid from permeating into the powder. Placing the assembled die in a cold isostatic press for compression molding, wherein the pressure of the cold isostatic press is 240MPa, the pressure maintaining time is 12min, and the pressure is relieved by adopting three-stage pressure relief to obtain a cold isostatic press composite blank;
sequentially carrying out internal oxidation (argon atmosphere, 900 ℃,4h), reduction (hydrogen atmosphere, 880 ℃, 8h) and sintering (hydrogen atmosphere, 980 ℃,4h) on the cold isostatic pressing composite blank, carrying out hot extrusion compounding (temperature is 960 ℃, heat preservation time is 3h, extrusion ratio is 12, diameter of the obtained extrusion rod is 20mm), removing head, tail and oxide skin from the hot extrusion compounded composite blank, carrying out cold drawing treatment on a chain type drawing machine, and finally carrying out saw cutting and straightening to obtain a composite bar with diameter of 16 mm;
the diameter of the composite bar is 13mm, the diameter of the core part is 8mm, and Al in the aluminum oxide dispersion strengthened copper alloy2O3The mass percentage content of (A) is 2.4%; the oxygen-free copper and aluminum oxide dispersion strengthened copper alloy composite interface has no layering, no bubbles and no inclusion;
and (3) performing hardness test on the composite bar according to GB/T230.1-2004 standard, and performing conductivity test on the composite bar according to YS/T478-2005 standard, wherein the test results comprise that the hardness of the oxygen-free copper is 63HRB, the hardness of the outer edge aluminum oxide dispersion strengthened copper alloy is 83HRB, and the overall conductivity is 91% IACS.
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and decorations can be made without departing from the principle of the present invention, and these modifications and decorations should also be regarded as the protection scope of the present invention.
Claims (3)
1. The preparation method of the composite bar is characterized by comprising the following steps:
mixing copper-aluminum alloy powder and cuprous oxide to obtain a mixture;
fixing an oxygen-free copper bar at the center of a cold isostatic pressing die, uniformly filling the mixture around the oxygen-free copper bar, and carrying out cold isostatic pressing to obtain a cold isostatic pressing composite blank;
sequentially carrying out heat treatment, hot extrusion compounding and drawing straightening on the cold isostatic pressing composite blank to obtain a composite bar;
the heat treatment comprises internal oxidation, reduction and sintering which are sequentially carried out;
the composite bar comprises a core and a skin;
the core part is made of oxygen-free copper;
the outer skin is made of aluminum oxide dispersion strengthened copper alloy;
the preparation method of the copper-aluminum alloy powder is a water atomization method or a nitrogen atomization method;
the mass percentage of aluminum in the copper-aluminum alloy powder is 0.1-1.2%;
the granularity of the copper-aluminum alloy powder is-100 meshes;
the pressure of the cold isostatic pressing is 180-240 MPa, the pressure maintaining time is 5-30 min, and three-stage pressure relief is adopted for pressure relief;
the internal oxidation is carried out in an argon atmosphere, the temperature is 850-900 ℃, and the heat preservation time is 2-4 h;
the reduction is carried out in a hydrogen atmosphere, the temperature is 820-880 ℃, and the heat preservation time is 4-8 h;
the sintering is carried out in a hydrogen atmosphere, the temperature is 900-980 ℃, and the heat preservation time is 2-4 h;
the temperature of hot extrusion compounding is 900-960 ℃, the heat preservation time is 1-3 h, and the extrusion ratio is 10-30 mm;
the diameter of the extrusion rod obtained after hot extrusion compounding is 13-25 mm;
the mass percentage of the alumina in the alumina dispersion strengthened copper alloy is 0.2-2.4%.
2. The method according to claim 1, wherein the ratio of the diameter of the core to the diameter of the composite rod is (3-9): (8-20);
and the diameter of the composite rod is greater than the diameter of the core.
3. The method of claim 1 wherein the oxygen-free copper is under the designation TU0, TU1, or TU 2.
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