High-strength high-plasticity cu / al2o3 laminated composite plate

By combining the embedded oxidation method and the rolling process with annealing, a high-strength and high-plasticity Cu/Al2O3 layered composite plate was prepared, which solved the problem of difficulty in balancing strength and plasticity in traditional methods and is suitable for large-scale industrial production.

CN116765129BActive Publication Date: 2025-12-12JIANGXI UNIV OF SCI & TECH +1
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Patent Information

Application Number
CN202310673022.3
Authority / Receiving Office
CN · China
Patent Type
Patents(China)
Current Assignee / Owner
Filing Date
2023-06-08
Publication Date
2025-12-12
Estimated Expiration
2043-06-08

AI Technical Summary

Technical Problem

Existing technologies struggle to improve the plasticity of Al2O3 particle-reinforced copper matrix composites while maintaining high strength, and traditional preparation methods are cumbersome and cannot meet the needs of large-scale industrial production and large-size composite material sheets.

Method used

Al2O3 dispersion-strengthened alloy plates were prepared by embedded internal oxidation method and combined with pure copper plates by a rolling process. The annealing temperature and rolling passes were controlled to form an alternating coarse and fine grain structure. Combined with the annealing process, the comprehensive mechanical properties of the material were improved.

Benefits of technology

It achieves a balance between high strength and high plasticity, making it suitable for industrial production of large-size Cu/Al2O3 layered composite plates. This simplifies the preparation process, reduces costs, and broadens the application areas.

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Abstract

The application discloses a high-strength and high-plasticity Cu / Al2O3 layered composite plate and a preparation method thereof. The high-strength and high-plasticity Cu / Al2O3 layered composite plate takes a pure copper plate and a copper-aluminum alloy plate as raw materials, the copper-aluminum alloy plate is made into an Al2O3 dispersion strengthened alloy plate through an embedding internal oxidation method, the Al2O3 dispersion strengthened alloy plate and the pure copper plate are obtained into a laminated base plate through a laminated mode, and the laminated base plate is prepared through a plurality of laminating and annealing. The Al2O3 dispersion strengthened alloy plate is prepared through the embedding internal oxidation method, the laminating pass is reasonably set, the Cu / Al2O3 layered composite plate is prevented from being cracked, the Cu / Al2O3 layered composite plate maintains a layered structure, and the laminated material can still maintain high plasticity after annealing while obtaining high strength.
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Description

TECHNICAL FIELD

[0001] The application relates to the technical field of new materials, in particular to a high-strength and high-plasticity Cu / Al2O3 layered composite plate and a preparation method thereof. BACKGROUND

[0002] There are various preparation methods for Al2O3 particle reinforced copper-based composite materials, and a traditional Al2O3 particle adding method is a simple and economical preparation method, but due to poor wettability between the matrix and the reinforcing body, the Al2O3 dispersoids tend to aggregate, so that the plasticity of the material is greatly limited while the strength is obtained. The process method for preparing the Al2O3 particle reinforced copper-based composite material by adopting a ball milling mixing internal oxidation method to reduce and prepare Al2O3 powder material and then performing hot-pressing sintering is often unable to perform large-scale industrial production due to complicated steps, and the prepared sample size specification is small, which is difficult to meet the industrial demand of large specification, large size and composite material plate. SUMMARY

[0003] The application aims to provide a high-strength and high-plasticity Cu / Al2O3 layered composite plate which can have high strength while still maintaining high plasticity and a preparation method thereof, and the specific technical scheme is as follows:

[0004] A high-strength and high-plasticity Cu / Al2O3 layered composite plate takes a pure copper plate and a copper-aluminum alloy plate as raw materials, the copper-aluminum alloy plate is made into an Al2O3 dispersion strengthened alloy plate through an embedding internal oxidation method, the dispersion strengthened alloy plate and the pure copper plate are obtained into a laminated base plate through laminating, and the laminated base plate is prepared after annealing through a plurality of laminating times.

[0005] Further, the mass percentage of aluminum in the copper-aluminum alloy plate is between 0.1 and 5.0%.

[0006] The application further discloses a preparation method of the high-strength and high-plasticity Cu / Al2O3 layered composite plate, mainly including the following steps:

[0007] (1) cleaning the surface of the copper-aluminum alloy plate to remove surface oxide film and oil stains and polishing;

[0008] (2) laying cuprous oxide powder on the bottom of a container, putting the copper-aluminum alloy plate into the container, and completely covering the copper-aluminum alloy plate with the cuprous oxide powder;

[0009] (3) putting the container into a tube furnace, vacuumizing, introducing a protective gas, vacuumizing again, introducing the protective gas again, heating to 700 DEG C to 1000 DEG C, keeping the temperature for not less than 30 minutes, and naturally cooling to obtain the Al2O3 dispersion strengthened alloy plate;

[0010] (4) removing the surface oxide film of the annealed pure copper plate, cleaning, polishing and laminating with the Al2O3 dispersion strengthened alloy plate to obtain the high-strength and high-plasticity Cu / Al2O3 layered composite plate.

[0011] (5) the pure copper plate and the Al2O3 dispersion strengthened alloy plate are first laminated to obtain a laminated base plate;

[0012] (6) the laminated base plate is cut into two plates of the same size and is laminated again to obtain a laminated plate;

[0013] (7) the laminated plate is cut and laminated for several times to obtain a Cu / Al2O3 layered composite plate;

[0014] (8) the Cu / Al2O3 layered composite plate is annealed to obtain a high-strength and high-plasticity Cu / Al2O3 layered composite plate.

[0015] Further, the first laminating reduction rate in step (5) is not less than 60%; and the cumulative laminating reduction rate is between 40% and 80%.

[0016] Further, the annealing temperature of the pure copper plate in step (4) is 500°C.

[0017] Further, the heating rate in step (3) is between 5 and 100 ℃ / min. Further, the annealing process in step (6) is: keeping at 200-700°C for 1-8 h.

[0018] The high-strength and high-plasticity Cu / Al2O3 layered composite plate of the application is prepared by the embedding internal oxidation method, which is beneficial to the preparation of large-size plates required by the industry. The laminated base plate is obtained by laminating with a pure copper plate, and the laminated base plate is laminated for several times. By controlling the annealing temperature, the pure Cu layer is recovered and recrystallized, while the Al2O3 dispersion strengthened alloy plate maintains the grains with the rolling deformation orientation, so that the material maintains high strength and high plasticity. After cumulative laminating, the material can still maintain high plasticity. BRIEF DESCRIPTION OF DRAWINGS

[0019] Figure 1 It is a schematic diagram of the coarse and fine crystal alternating distribution of the high-strength and high-plasticity Cu / Al2O3 layered composite plate in Example 1.

[0020] Figure 2 It is a mechanical property curve diagram of the high-strength and high-plasticity Cu / Al2O3 layered composite plate in Example 1.

[0021] Figure 3 It is a mechanical property curve diagram of the high-strength and high-plasticity Cu / Al2O3 layered composite plate in Example 2. IMPLEMENTATION

[0022] The application will be described more fully hereinafter with reference to the accompanying drawings, in which embodiments of the application can take many different forms. The application should not be construed as limited to the embodiments set forth herein. As such, the following embodiments are illustrative rather than limiting in nature. Example 1

[0023] The specific steps are shown as follows

[0024] (1) Grind the 1mm thick copper-aluminum alloy plate to remove the surface oxide film.

[0025] (2) Put the ground plate into a crucible containing cuprous oxide powder, and try to ensure that the plate is in the middle of the crucible; other high-temperature resistant containers can also be used.

[0026] (3) Put the crucible into a tube furnace, vacuumize, and introduce a protective gas such as argon; after reaching normal pressure, vacuumize again, and then introduce argon, heat to 950°C at a rate of 5°C / min and keep for 8h, then take out the plate after the tube furnace cools naturally, to obtain an Al2O3 dispersion strengthened alloy plate.

[0027] (4) Cut the 1mm thick pure Cu plate after annealing at 500°C to the same size as the Al2O3 dispersion strengthened alloy plate. Sand the surface of the plate to remove the oxide film, then clean the surface of the plate with alcohol, and use a brush to polish the surface of the plate.

[0028] (5) Stack the three plates in the order of copper plate-Al2O3 dispersion strengthened alloy plate-copper plate.

[0029] (6) Put the stacked plates into the rolling mill for rolling at a reduction ratio of 65%.

[0030] (7) First, shear and flatten the unstable head and tail of the rolled plate, then divide the plate into two, and try to ensure that two plates of the same size are obtained.

[0031] (8) Put the stacked plates into the rolling mill for rolling at a reduction ratio of 55%.

[0032] (9) Repeat steps (6)-(8) nine times.

[0033] The above process can be used to prepare Cu / Al2O3 layered composite plates with different layer thicknesses after 1, 3, 5, 7, and 9 passes of stacking and rolling. The plate obtained after 9 passes of stacking and rolling has a strength of 586MPa, an elongation of 10%, and an electrical conductivity of 73%IACS. Example 2

[0034] The specific steps are shown as follows:

[0035] (1) Grind the 1mm thick copper-aluminum alloy plate to remove the surface oxide film.

[0036] (2) Put cuprous oxide powder on the bottom of the container, put the copper-aluminum alloy plate into the container, and then cover it completely with cuprous oxide powder.

[0037] (3) Put the crucible into the tube furnace, vacuumize, pass protective gas, vacuumize again, pass protective gas again, heat to 950°C and keep for 8 hours, take out the plate after the tube furnace is naturally cooled, and get the Al2O3 dispersion strengthened alloy plate.

[0038] (4) Cut the pure Cu plate to the same size as the Al2O3 dispersion strengthened alloy plate after annealing at 500°C. Grind the surface of the plate with sandpaper to remove the oxide film, then clean the surface of the plate with alcohol, and fully polish the surface of the plate with a brush to ensure good interface bonding.

[0039] (5) Stack the three plates in the order of Cu plate-Al2O3 dispersion strengthened alloy plate-Cu plate.

[0040] (6) Put the stacked plates into the rolling mill for rolling with a reduction ratio of 65%.

[0041] (7) First, shear and flatten the unstable head and tail of the rolled plate, then divide the plate into two, and try to ensure that the two plates are of the same size.

[0042] (8) Put the stacked plates into the rolling mill for rolling with a reduction ratio of 50%.

[0043] (9) Repeat steps (6)-(8) nine times.

[0044] After nine times of accumulative rolling, take several samples from the same plate, and then anneal at 200°C, 300°C, 400°C, 500°C, 600°C, and 700°C for 1 hour, respectively. The plate obtained after annealing at 300°C for 1 hour has a strength of 423 MPa, an elongation of 25%, and an electrical conductivity of 80% IACS. The plate obtained after annealing at 400°C for 1 hour has a strength of 413 MPa, an elongation of 30%, and an electrical conductivity of 85% IACS. The high-strength and high-plasticity material has similar comprehensive performance and matched strength and plasticity. Example 3

[0045] The specific steps are as follows:

[0046] (1) Grind the 1 mm thick copper-aluminum alloy plate to remove the surface oxide film.

[0047] (2) Put cuprous oxide powder on the bottom of the container, put the copper-aluminum alloy plate into the container, and then cover it completely with cuprous oxide powder.

[0048] (3) Put the crucible into the tube furnace, vacuumize, pass the protective gas, vacuumize again, pass the protective gas again, and heat the Cu-Al alloy at 700℃, 800℃, 900℃ and 950℃ respectively for 8 hours. After the tube furnace is naturally cooled, the plate is taken out, and the Al2O3 dispersion strengthened alloy plate is obtained.

[0049] (4) Cut the 1mm thick pure Cu plate after annealing to the same size of the Al2O3 dispersion strengthened alloy plate. Grind the surface of the plate with sandpaper to remove the oxide film, then clean the surface of the plate with alcohol, and polish the surface of the plate with a brush.

[0050] (5) Stack the three plates in the order of copper plate-Al2O3 dispersion strengthened alloy plate-copper plate.

[0051] (6) Put the stacked plates into the rolling mill for rolling, with a reduction rate of 60%.

[0052] (7) First, shear and flatten the unstable head and tail of the rolled plate, then divide the plate into two, and try to ensure that the two plates are of the same size; stack the two plates.

[0053] (8) Put the stacked plates into the rolling mill for rolling, with a reduction rate of 50%.

[0054] (9) Repeat steps (6)-(8) three times.

[0055] After 3 passes of stacking and rolling, the Cu / Al2O3 layered composite plate is prepared, wherein the Al2O3 dispersion strengthened alloy plate prepared by the 700℃ embedding internal oxidation method and the pure Cu plate have a strength of 400MPa and an elongation of 11% after 3 passes of stacking and rolling; the Al2O3 dispersion strengthened alloy plate prepared by the 800℃ embedding internal oxidation method and the pure Cu plate have a strength of 415MPa and an elongation of 10% after 3 passes of stacking and rolling; the Al2O3 dispersion strengthened alloy plate prepared by the 900℃ embedding internal oxidation method and the pure Cu plate have a strength of 469MPa and an elongation of 9% after 3 passes of stacking and rolling; the Al2O3 dispersion strengthened alloy plate prepared by the 950℃ embedding internal oxidation method has a strength of 475MPa and an elongation of 8% after 3 passes of stacking and rolling.

[0056] The above embodiments can prepare large-size plates required by industry by using the embedding internal oxidation method, and it is convenient to carry out subsequent accumulative roll bonding. Rolling is a process of large plastic deformation, which can improve the strength of the material, but the plasticity of the material will be significantly reduced; by adjusting the bonding passes, the material obtains the optimal mechanical properties, and subsequent annealing processes at different temperatures are used to make the material obtain the comprehensive mechanical properties of high strength and high plasticity. After annealing, the material in embodiments 2 and 3 first recrystallizes in the Cu layer of the plate, and the grains grow again; the Al2O3 dispersion strengthened alloy layer is hindered from moving due to the second phase particles, so that the grain growth is inhibited, thereby achieving the structure of alternating coarse and fine grains, and further achieving the compatibility of strength and plasticity. In addition, the process method of the application is used to prepare the high-strength and high-plasticity Cu / Al2O3 laminated composite plate, which is simple to operate and low in cost, and therefore is extremely beneficial to industrial production, and this preparation method greatly widens the application field of the Al2O3 copper-based composite material.

[0057] The above examples are only used to illustrate the application, and in addition, there are various different embodiments, which can be thought of by those skilled in the art after understanding the idea of the application, and therefore, they will not be listed one by one here.

Claims

1. A method for preparing high-strength high-ductility Cu / Al2O3 laminated composite sheet material, characterized in that, The application relates to a method for preparing a Cu / Al2O3 layered composite plate, which comprises the following steps of using pure copper plate and copper-aluminum alloy plate as raw materials, cleaning the surface of the copper-aluminum alloy plate to remove surface oxide film and oil stains, polishing, laying cuprous oxide powder on the bottom of a container, putting the copper-aluminum alloy plate into the container, and completely covering the copper-aluminum alloy plate with the cuprous oxide powder, putting the container into a tubular furnace, vacuumizing, introducing protective gas, vacuumizing again, introducing protective gas again, heating to 700-1000 DEG C, keeping the temperature for not less than 30 minutes, naturally cooling, removing surface oxide film from the annealed pure copper plate, cleaning and polishing, first rolling the pure copper plate and the Al2O3 dispersion strengthened alloy plate into a laminated base plate, cutting the laminated base plate into two plates with the same size, and rolling again to obtain a laminated plate, cutting and laminating the laminated plate for several times to obtain the Cu / Al2O3 layered composite plate, and annealing the Cu / Al2O3 layered composite plate to obtain a high-strength and high-plasticity Cu / Al2O3 layered composite plate. The mass percentage of aluminum in the copper-aluminum alloy plate is 0.1-5.0%. The annealing temperature of the pure copper plate in step (4) is 400-700 DEG C. The heating rate in step (3) is 5-100 DEG C / min. The annealing process in step (8) is 200-700 DEG C for 1-8 h. ​ ​ ​ ​ 2. The production method according to claim 1, wherein ​ 3. The production method according to claim 1, wherein ​ 4. The production method according to claim 1, wherein ​ 5. The production method according to claim 1, wherein ​

Citation Information

Patent Citations

  • High-strength high-conduction strengthened dispersion copper alloy and preparation method thereof

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