CN112588856B - Preparation method of high-performance Cu-Ni-Al alloy plate strip - Google Patents
Preparation method of high-performance Cu-Ni-Al alloy plate strip Download PDFInfo
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- CN112588856B CN112588856B CN202011530004.2A CN202011530004A CN112588856B CN 112588856 B CN112588856 B CN 112588856B CN 202011530004 A CN202011530004 A CN 202011530004A CN 112588856 B CN112588856 B CN 112588856B
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B21—MECHANICAL METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL; PUNCHING METAL
- B21C—MANUFACTURE OF METAL SHEETS, WIRE, RODS, TUBES OR PROFILES, OTHERWISE THAN BY ROLLING; AUXILIARY OPERATIONS USED IN CONNECTION WITH METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL
- B21C23/00—Extruding metal; Impact extrusion
- B21C23/001—Extruding metal; Impact extrusion to improve the material properties, e.g. lateral extrusion
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
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- C22C9/00—Alloys based on copper
- C22C9/01—Alloys based on copper with aluminium as the next major constituent
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- 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 provides a preparation method of a high-performance Cu-Ni-Al alloy plate strip, belonging to the field of forming processing of non-ferrous metal thin strips; the method comprises the following steps: preparing a raw material containing Cu, Ni and Al components according to a certain mass ratio, smelting to obtain a melt, preparing a forging stock sample by hot rolling, performing equal-channel extrusion deformation treatment, recrystallization annealing, rapid deformation and annealing treatment; the method can refine the crystal grains through equal channel angular extrusion and recrystallization annealing, can form nano-scale twin crystals through rapid deformation and annealing treatment on the basis of grain refinement, separates out nano-scale second-phase particles, obviously improves the performance of the alloy, and prepares the high-performance Cu-Ni-Al alloy strip.
Description
Technical Field
The invention belongs to the field of forming processing of non-ferrous metal thin strips, and relates to a method for processing a high-performance copper alloy plate strip, in particular to a method for preparing a high-performance Cu-Ni-Al alloy plate strip.
Background
Copper and its alloy have good electric and thermal conductivity, and high plasticity and toughness, so that they are widely used as high-conductivity materials. In recent years, with rapid development of economy, particularly rapid development of electronic communication and rail transit, higher demands are made on the performance of copper alloys.
In recent years, in order to obtain a copper alloy having more excellent mechanical properties, materials researchers have made a new material having a nanocrystalline structure by severe plastic deformation, and then have advanced the properties of the material by introducing a precipitated phase into the matrix by aging treatment after deformation and further superimposing the precipitated phase on the nanocrystalline structure. This research has led to a series of great efforts, such as the multi-directional forging followed by the aging treatment of CuCrZr alloy, which can reach 650MPa of tensile strength. As is well known, nano twin crystal materials are a special structure with various excellent properties, such as excellent strength and plasticity, excellent thermal stability, ultrahigh electrical conductivity, and the like. Therefore, nano twinning strengthening has natural performance advantages in combination with age-induced precipitation strengthening. By the method, the copper alloy material with more excellent mechanical property is hopeful to be prepared.
Disclosure of Invention
The invention overcomes the defects of the prior art and provides a preparation method of a high-performance Cu-Ni-Al alloy plate strip to improve the performance of a copper alloy.
In order to achieve the above object, the present invention is achieved by the following technical solutions.
A preparation method of a high-performance Cu-Ni-Al alloy plate strip comprises the following steps:
1) the materials are mixed according to the mass ratio of Cu to Ni to Al =90-94:1-5: 3-7.
2) Smelting the proportioned raw materials to obtain a Cu-Ni-Al alloy melt; and casting an ingot on the Cu-Ni-Al alloy melt and carrying out homogenization annealing to prepare a sample.
3) And (3) carrying out equal channel extrusion deformation treatment on the forging stock sample, namely putting the sample into an equal channel angular extrusion die, preheating the die, and then extruding the sample at the speed of 18-22 mm/s.
4) And (3) carrying out recrystallization annealing treatment on the sample subjected to the equal channel angular extrusion, wherein the recrystallization annealing temperature is 650-700 ℃, and the time is 50-70 min.
5) Rapidly deforming the sample subjected to recrystallization annealing at a deformation rate of 103/s。
6) And annealing the rapidly deformed sample to obtain the Cu-Ni-Al alloy plate strip.
Preferably, in the step 1, the materials are mixed according to the mass ratio of Cu to Ni to Al =92 to 3 to 5.
Preferably, in step 3, the sample is placed into an equal channel angular extrusion die to be subjected to multi-pass extrusion deformation, the sample is reduced at the speed of 20mm/s by a vertical hydraulic press, and the sample is rotated 90 degrees in a counterclockwise direction along the reduction direction as an axis after each pass of extrusionoAnd carrying out next-pass extrusion.
Preferably, the inner angle of the equal channel angle extrusion die is 90 degrees, and the outer angle is 37 degrees; strain after each extrusion, e = 0.992.
Preferably, the sample after the equal-diameter angle extrusion recrystallization annealing is quickly deformed by a Hopkinson bar, and the deformation rate is 103/s。
Further, the deformation amount was 80%.
Preferably, in the step 2, the proportioned raw materials are subjected to vacuum induction melting with the vacuum degree of 10-2Pa。
Preferably, the vacuum induction melting comprises the following specific steps: firstly adding electrolytic Cu, smelting at 1300 ℃, then sequentially adding pure nickel and pure aluminum, and fully smelting and stirring to obtain a Cu-Ni-Al alloy melt.
Preferably, in the step 2, the Cu-Ni-Al alloy melt is poured into a water-cooling metal mold at the temperature of 1200-1300 ℃, and is cooled and solidified into an ingot blank.
Preferably, the annealing in step 6 is performed in a vacuum heat treatment furnace, wherein the annealing temperature is 450 ℃ and the annealing time is 30 min.
Compared with the prior art, the invention has the beneficial effects that.
The invention designs and develops a Cu-Ni-Al alloy, and obtains a high-performance Cu-Ni-Al alloy plate strip through design optimization of alloy components and a series of measures such as multidirectional forging, recrystallization annealing, rapid deformation, annealing and the like.
1. The alloy fault energy is made to be 78mJ/m of pure copper by adding 7.5 mass percent of aluminum into the copper2Reduced to 8mJ/m2Reducing the stacking fault energy will significantly increase the probability of twinning during deformation. Ni is formed by adding 3.0 mass percent of nickel and a part of aluminum element3Al and NiAl precipitated phases strengthen the alloy performance.
2. Meanwhile, grains can be refined through equal channel angular extrusion and recrystallization annealing, nano-scale twin crystals can be formed through rapid deformation and annealing treatment on the basis of grain refinement, nano-scale second phase particles are separated out, and the performance of the alloy is remarkably improved. And preparing the high-performance Cu-Ni-Al alloy plate strip.
3. And obtaining refined grains with the average grain size of below 10 mu m by multi-directional forging and recrystallization annealing to generate fine-grain strengthening effect.
4. On the basis of grain refinement, 10 times3Rapid Hopkinson bar annealing heat treatment of/s to obtain nano-scale Ni3Al and NiAl precipitation strengthening phases and 3-5nm nanoscale twin crystals to strengthen a matrix.
According to the invention, a precipitated phase is introduced into the nano twin crystal Cu-Ni-Al alloy, so that an alloy strip with more excellent mechanical properties is obtained.
Drawings
In order to make the technical problems, technical solutions and beneficial effects to be solved by the present invention more clearly understood, the following drawings are combined for description:
FIG. 1 is a schematic view of an isometric extruded block according to an embodiment;
FIG. 2 is a schematic view of an equal channel angular extrusion die of an embodiment;
FIG. 3 is a schematic view of a selected extrusion path of an embodiment;
FIG. 4 is a diagram of the phase of gold after isodiametric extrusion + recrystallization annealing of the examples;
FIG. 5 is a diagram of a fast deforming Hopkinson bar apparatus of an embodiment;
FIG. 6 is a metallographic picture of a sample after rapid deformation according to the example;
FIG. 7 is a high-resolution transmission photograph (deformation twinning) of the sample after rapid deformation according to the example;
in the figure, 1 is a die, 2 is a forged sample, 3 is a punch, 5 is a bullet, 6 is a parallel light source, 7 is an input rod, 8 is an output rod, 9 is an absorption rod, 10 is a damper, 11 is an amplifier, 12 is a time measuring instrument, 13 is a waveform memory, 14 is a data processing system, 15 is a super dynamic strain gauge, and 16 is a resistance strain gauge.
Detailed Description
In order to make the technical problems, technical solutions and advantageous effects to be solved by the present invention more clearly apparent, the present invention is further described in detail with reference to the embodiments and the accompanying drawings. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention. The technical solution of the present invention is described in detail below with reference to the embodiments and the drawings, but the scope of protection is not limited thereto.
A preparation method of a high-performance Cu-Ni-Al alloy plate strip comprises the following steps:
1) preparing materials: weighing cathode pure copper, industrial pure nickel and industrial pure aluminum according to the mass ratio of Cu to Ni to Al =92:3.0: 5.0.
2) Vacuum induction melting: the alloy is subjected to vacuum induction melting with the vacuum degree of 10-2Pa, firstly adding electrolytic copper, wherein the smelting temperature is 1300 ℃, quickly smelting the electrolytic copper, sequentially adding pure nickel and pure aluminum through a feeding bin when the alloy is basically molten, and fully smelting and stirring to obtain a Cu-Ni-Al alloy melt;
3) casting an ingot: pouring the copper alloy melt into a water-cooling metal die at a set temperature (about 1250 ℃), and cooling and solidifying the copper alloy melt into an ingot blank.
4) Homogenizing and annealing: homogenizing the copper alloy cast ingot in a vacuum annealing furnace with the vacuum degree of 10-1Pa, homogenizing annealing temperature 800 deg.C, and time 4 h.
5) Face milling: removing surface scale by milling;
6) equal-channel extrusion deformation treatment: and cutting the homogenized and annealed blank into a sample of 30mm multiplied by 24mm multiplied by 20mm, putting the sample into an equal-diameter angular extrusion die for extrusion deformation, wherein the internal angle phi of the die is 90 degrees, and the external angle phi of the die is 37 degrees. MoS used for die before extrusion2The mixed liquid of the lubricating oil and the engine oil is used as a lubricant to fully lubricate a pressure head and an extrusion channel through vertical hydraulic pressureThe machine presses down the sample at a speed of 20mm/s, and rotates the sample 90 degrees counterclockwise along the pressing direction as an axis after each time of one-pass extrusiono（BCPath) for the next extrusion pass. The extrusion was carried out continuously in 8 passes. Engineering strain epsilon =0.992 per reduction. The 8-pass extrusion co-cumulative strain s = 7.936. A schematic of the equal channel extrusion sample is shown in fig. 1, and a schematic of the die extrusion and selected path diagrams are shown in fig. 2 and 3.
7) And (3) recrystallization annealing: placing the multi-directionally forged sample in a vacuum annealing furnace for recrystallization annealing treatment, wherein the vacuum degree of the vacuum annealing furnace is 10-1Pa, the recrystallization annealing temperature is 680 ℃, and the time is 1 h. The average grain size after recrystallization annealing is 1.3 to 3 μm. The annealed sample is shown in fig. 4.
8) Quick cold deformation: the aging sample is quickly deformed on quick deformation equipment such as a Hopkinson bar and the like, and the deformation rate is 103And s. The thickness of the sample is changed from 9mm to 1.8mm, the deformation is 80%, and thus the deformation twin size is 10nm, and the twin percentage is 85%. The schematic diagram of the apparatus is shown in fig. 5, and the gold phase diagram and the transmission diagram of the deformed sample are shown in fig. 6 and 7.
9) And (3) annealing treatment: and (3) annealing the rapid deformation sample in a vacuum heat treatment furnace, wherein the annealing temperature is 450 ℃, the annealing time is 30min, the total volume fraction of deformation twin crystals and annealing twin crystals is 70%, and nano precipitated phases are dispersed and distributed near twin crystal boundaries and dislocation lines and are 10 nm.
The hardness value of the obtained copper alloy is measured by a Vickers hardness meter, the conductivity is measured by a conductivity meter, and the tensile strength, the yield strength and the elongation are tested by a microcomputer-controlled electronic universal testing machine. The mechanical properties of the final high-strength high-conductivity copper alloy are as follows: 340 HV; the conductivity is 13%; tensile strength is 1014 MPa; yield strength 978 Mpa; the elongation is 12%.
Adding 7.5 mass percent of aluminum into copper to ensure that the alloy fault energy is 78mJ/m of that of pure copper2Reduced to 8mJ/m2Reducing the stacking fault energy will significantly increase the probability of twin formation during deformation. Ni is formed by adding 3.0 wt% of nickel and a part of aluminum element3Al and NiAl precipitate precipitated phases strengthen the alloy performance. Refined grains with the average grain size of below 10 mu m are obtained through multidirectional forging and recrystallization annealing, and a fine-grain strengthening effect is generated. On the basis of grain refinement, 10 times3Rapid Hopkinson bar annealing heat treatment of/s to obtain nano-scale Ni3Al and NiAl precipitation strengthening phases and 3-5nm nanometer twin crystals to strengthen the matrix.
While the invention has been described in further detail with reference to specific preferred embodiments thereof, it will be understood by those skilled in the art that various changes in form and details may be made therein without departing from the spirit and scope of the invention as defined by the appended claims.
Claims (7)
1. A preparation method of a high-performance Cu-Ni-Al alloy plate strip is characterized by comprising the following steps:
1) proportioning according to the mass ratio of Cu to Ni to Al =92 to 3 to 5;
2) smelting the proportioned raw materials to obtain a Cu-Ni-Al alloy melt; casting and ingot casting are carried out on the Cu-Ni-Al alloy melt, and a sample is prepared by homogenizing annealing;
3) performing equal channel extrusion deformation treatment on the sample, namely preheating an equal channel angular extrusion die, putting the sample into the equal channel angular extrusion die for multi-pass extrusion deformation, wherein the multi-pass extrusion deformation is to press down the sample at the speed of 20mm/s by using a vertical hydraulic press, and after each pass of extrusion, rotating the sample 90 degrees counterclockwise along the pressing direction as an axisoCarrying out extrusion of the next pass; the inner angle of the equal-diameter angle extrusion die is 90 degrees, and the outer angle is 37 degrees; strain after each extrusion, e = 0.992;
4) carrying out recrystallization annealing treatment on the sample subjected to the equal channel angular extrusion, wherein the recrystallization annealing temperature is 650-700 ℃, and the time is 50-70 min;
5) the sample after recrystallization annealing is rapidly deformed with the deformation rate of 103/s；
6) Annealing the rapidly deformed sample to obtain a Cu-Ni-Al alloy plate strip; the annealing temperature is 450 ℃, and the annealing time is 30 min.
2. The method for preparing the high-performance Cu-Ni-Al alloy plate strip according to claim 1, wherein a sample subjected to radial angle extrusion recrystallization annealing is subjected to rapid deformation by using a Hopkinson bar at a deformation rate of 103/s。
3. The method for producing a high-performance Cu-Ni-Al alloy sheet strip according to claim 2, wherein the deformation amount is 80%.
4. The method for preparing a high-performance Cu-Ni-Al alloy strip according to claim 1, wherein in the step 2), the proportioned raw materials are subjected to vacuum induction melting with the vacuum degree of 10-2Pa。
5. The method for preparing the high-performance Cu-Ni-Al alloy plate strip according to claim 4, wherein the vacuum induction melting comprises the following specific steps: firstly adding electrolytic Cu, smelting at 1300 ℃, then sequentially adding pure nickel and pure aluminum, and fully smelting and stirring to obtain a Cu-Ni-Al alloy melt.
6. The method for preparing a high-performance Cu-Ni-Al alloy strip as claimed in claim 5, wherein in the step 2), the Cu-Ni-Al alloy melt is poured into a water-cooled metal mold at 1200-1300 ℃, and cooled and solidified into an ingot blank.
7. The method for manufacturing a high-performance Cu-Ni-Al alloy strip according to claim 1, wherein the annealing in the step 6) is performed in a vacuum heat treatment furnace.
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