CN117702022A - Preparation method of composite isomerism pure copper with grain double peak and gradient structure - Google Patents
Preparation method of composite isomerism pure copper with grain double peak and gradient structure Download PDFInfo
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- CN117702022A CN117702022A CN202410083901.5A CN202410083901A CN117702022A CN 117702022 A CN117702022 A CN 117702022A CN 202410083901 A CN202410083901 A CN 202410083901A CN 117702022 A CN117702022 A CN 117702022A
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- isomerism
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- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 title claims abstract description 74
- 229910052802 copper Inorganic materials 0.000 title claims abstract description 74
- 239000010949 copper Substances 0.000 title claims abstract description 74
- 239000002131 composite material Substances 0.000 title claims abstract description 16
- 238000002360 preparation method Methods 0.000 title claims abstract description 16
- 238000005096 rolling process Methods 0.000 claims abstract description 19
- 238000000137 annealing Methods 0.000 claims abstract description 18
- 238000007709 nanocrystallization Methods 0.000 claims abstract description 12
- 238000000034 method Methods 0.000 claims abstract description 10
- 238000005422 blasting Methods 0.000 claims description 15
- 230000002902 bimodal effect Effects 0.000 claims description 10
- 238000005516 engineering process Methods 0.000 claims description 9
- 238000005498 polishing Methods 0.000 claims description 7
- 239000000758 substrate Substances 0.000 claims description 6
- 229910000831 Steel Inorganic materials 0.000 claims description 5
- 239000010959 steel Substances 0.000 claims description 5
- 239000013078 crystal Substances 0.000 claims description 2
- 239000000463 material Substances 0.000 abstract description 15
- 238000001953 recrystallisation Methods 0.000 abstract 1
- 230000000052 comparative effect Effects 0.000 description 12
- 239000002689 soil Substances 0.000 description 5
- 230000007246 mechanism Effects 0.000 description 3
- 238000004381 surface treatment Methods 0.000 description 3
- 230000002195 synergetic effect Effects 0.000 description 2
- 239000000956 alloy Substances 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 239000002178 crystalline material Substances 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000001125 extrusion Methods 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 238000005482 strain hardening Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000009864 tensile test Methods 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
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Abstract
The invention discloses a preparation method of composite isomerism pure copper with a grain double peak and gradient structure, and belongs to the technical field of material preparation. The method comprises the steps of firstly asynchronously rolling a purchased commercial anaerobic pure copper plate (T2), then carrying out short-time annealing treatment, and carrying out surface nanocrystallization treatment on the pure copper plate for 2 minutes in a room temperature environment to finally obtain the pure copper material with the composite heterostructure. The invention adopts the asynchronous rolling of pure copper plates with the total deformation of 33 percent at room temperature in advance, so that the pure copper plates have extensive recrystallization behavior in the subsequent annealing to form grain size difference (double-peak structure). The surface of the copper plate is treated to form a microstructure gradient along the core part of the plate, so that a double-peak gradient composite heterostructure is formed.
Description
Technical Field
The invention relates to a preparation method of composite isomerism pure copper with a grain double peak and gradient structure, belonging to the technical field of material preparation.
Background
Pure copper materials are widely used in various industries due to their excellent properties of plasticity, electrical conductivity, thermal conductivity, low cost, etc. Pure copper materials play an important role in the fields of electronic devices, mechanical manufacturing, aerospace, construction chemical industry and the like.
The strength and plasticity properties of metals have been a pair of performance requirements in materials science that are difficult to balance. Typically, the strength and plasticity of a material exhibit an "inverted" relationship, i.e., high strength often means low plasticity. In the current industrial production, the preparation method of the product is mainly based on the requirements of the working environment, but the preparation method often leads to obvious short plates of the material in terms of strength and plasticity, and limits the further development of the product.
Researchers have focused on the study of nanocrystalline and ultra-fine crystalline materials to overcome the problems. These materials exhibit high strength properties due to their homogeneous bulk structure. Further, the strength of the material can be further improved by large plastic deformation technology such as equal-diameter angular extrusion, asynchronous rolling and other means. However, the materials prepared by these methods tend to be relatively low in extensibility, limiting their versatility in practical applications.
Aiming at the problem, the invention provides a scheme of asynchronous rolling, short-time annealing and high-energy shot blasting surface treatment, and the composite pure copper plate with a grain double peak and gradient structure is successfully prepared. Compared with untreated pure copper plates, the mechanical property of the novel material is remarkably improved, high strength and hardness are maintained, and less plasticity is sacrificed. The optimized preparation method benefits from the synergistic effect of grain double peaks and microstructure gradient structures, the processing hardening capacity and the mutual coordination of various mechanisms, and the problem of abrupt performance change is effectively avoided. In addition, the method has the advantages of simple process flow, low equipment cost, good product reliability, high practical value and market prospect.
Disclosure of Invention
The invention aims to provide a preparation method of composite heterogeneous pure copper with a grain double-peak and gradient structure, which improves the toughness of the pure copper by changing microstructure firstly and improves the strength of the pure copper by surface treatment; the process has the advantages of low cost of required equipment, good product reliability and simple process flow, and comprises the following steps:
(1) Commercial oxygen-free pure copper plates of 6mm thickness were purchased and surface polished to remove the oxide layer.
(2) And (3) asynchronously rolling the pure copper plate with the thickness of 6mm obtained in the step (1) to 4mm in 3-5 times at room temperature, wherein the total deformation is 33%, and the speed ratio of the upper roller to the lower roller in the rolling process is 1.3.
(3) And (3) annealing the rolled pure copper plate at 450 ℃ for 15min to obtain a grain bimodal structure, and polishing the surface, and removing dirt for later use.
(4) And (3) carrying out surface nanocrystallization treatment on the pure copper substrate obtained in the step (3) in a room temperature environment, and finally obtaining the pure copper with double-peak crystal grain and composite isomerism of the gradient structure.
Preferably, in the step (3), the surface nanocrystallization treatment is to treat the surface by adopting a high-energy shot blasting technology, wherein the treatment time is 2min, the shot blasting rate is selected to be 30m/s, and the diameter of the steel ball is 8mm.
The invention has the beneficial effects that:
(1) The method comprises the steps of carrying out short-time annealing on an asynchronously rolled copper plate to form a grain bimodal structure, carrying out surface short-time treatment on the polished pure copper plate by using a high-energy shot blasting technology (a steel ball carries out high-speed bombardment on the pure copper surface), and obtaining the grain bimodal and gradient structure composite heterogeneous pure copper on the basis of grain bipeaking, wherein microstructure of the processed copper plate is distributed in a gradient manner from the surface to the center.
(2) The hard area and soft area of the grain double peaks, the surface structure and the core structure cooperate with each other and various deformation mechanisms are combined in the mechanical test stretching process, so that the mechanical property of pure copper is improved, the yield strength is improved, and meanwhile, good plasticity can be maintained.
Drawings
FIG. 1 is a comparison of the tensile curves of pure copper sheets obtained in the examples and comparative examples of the present invention and annealed raw samples at room temperature.
FIG. 2 is a diagram showing the structure of the double peaks of pure copper grains annealed at 450℃for 15min in example 1.
FIG. 3 is a graph showing the surface-to-core hardness of pure copper after annealing and high energy peening for 2 minutes in example 1.
Detailed Description
The invention will be described in further detail with reference to the drawings and the specific embodiments, but the scope of the invention is not limited to the description.
Example 1
The preparation method of the composite isomerism pure copper with the grain double peak and gradient structure comprises the following steps:
(1) Commercial oxygen-free pure copper plates of 6mm thickness were purchased and surface polished to remove the oxide layer.
(2) And (3) carrying out 3-5 times of asynchronous rolling on the pure copper plate with the thickness of 6mm obtained in the step (1) at room temperature to obtain the copper plate with the total deformation of 33%, wherein the speed ratio of the upper roller to the lower roller in the rolling process is 1.3.
(3) And (3) annealing the pure copper plate subjected to asynchronous rolling for 15min at 450 ℃ and polishing the surface and removing the soil.
(4) And (3) carrying out surface nanocrystallization treatment on the pure copper substrate obtained in the step (3) in a room temperature environment, adopting a high-energy shot blasting technology to treat the surface, wherein the shot blasting speed is 30m/s, the diameter of the steel ball is 8mm, and the treatment time is 2min.
The bimodal structure of the pure copper grains obtained in this example is shown in fig. 2, and it can be seen from the figure that recrystallized grains (soft zone) are surrounded by fine deformed grains after short annealing and that the recrystallized grains are significantly larger in size than the deformed grains.
The graph of the surface to core hardness of the pure copper obtained in this example is shown in fig. 3, and it can be seen from the graph that the surface to core hardness gradually decreases, which indicates that the microstructure has a gradient structure from the surface to the core, and the hardness difference of different regions in the bimodal structure is also shown by the larger core hardness error bar.
Comparative example 1
In contrast, this example differs from example 1 in that the annealing temperature and time are different, and the specific preparation steps are as follows:
(1) Commercial oxygen-free pure copper plates of 6mm thickness were purchased and surface polished to remove the oxide layer.
(2) And (3) carrying out 3-5 times of asynchronous rolling on the pure copper plate with the thickness of 6mm obtained in the step (1) at room temperature to obtain the copper plate with the total deformation of 33%, wherein the speed ratio of the upper roller to the lower roller in the rolling process is 1.3.
(3) And (3) annealing the rolled pure copper plate at 700 ℃ for 2 hours, and polishing the surface and removing the soil.
(4) And (3) carrying out short-time surface nanocrystallization treatment on the pure copper substrate obtained in the step (3) in a room temperature environment, and treating the surface by a high-energy shot blasting technology, wherein the shot blasting rate is selected to be 30m/s, the diameter is 8mm, and the treatment time is 2min.
Comparative example 2
In contrast, this example differs from example 1 in that the annealing temperature and time are different, and the specific preparation steps are as follows:
(1) Commercial oxygen-free pure copper plates of 6mm thickness were purchased and surface polished to remove the oxide layer.
(2) And (3) carrying out 3-5 times of asynchronous rolling on the pure copper plate with the thickness of 6mm obtained in the step (1) at room temperature to obtain the copper plate with the total deformation of 33%, wherein the speed ratio of the upper roller to the lower roller in the rolling process is 1.3.
(3) And (3) annealing the rolled pure copper plate at 350 ℃ for 30min, and polishing the surface and removing the soil.
(4) And (3) carrying out short-time surface nanocrystallization treatment on the pure copper substrate obtained in the step (3) in a room temperature environment, and treating the surface by a high-energy shot blasting technology, wherein the shot blasting rate is selected to be 30m/s, the diameter is 8mm, and the treatment time is 2min.
Comparative example 3
The difference between this example and example 1 as a comparison is that asynchronous rolling is not performed, and the specific preparation steps are as follows:
(1) Commercial oxygen-free pure copper plates of 6mm thickness were purchased and surface polished to remove the oxide layer.
(2) And (3) annealing the pure copper plate processed in the step (1) at 450 ℃ for 15min, and polishing the surface and removing the soil.
(3) And (3) carrying out surface nanocrystallization treatment on the pure copper substrate obtained in the step (2) in a room temperature environment, adopting a high-energy shot blasting technology to treat the surface, wherein the shot blasting speed is 30m/s, the diameter of the steel ball is 8mm, and the treatment time is 2min.
Comparative example 4
As a comparison, this example differs from example 1 in that the surface is not treated by the high energy peening technique, and the specific preparation steps are as follows:
(1) Commercial oxygen-free pure copper plates of 6mm thickness were purchased and surface polished to remove the oxide layer.
(2) And (3) carrying out 3-5 times of asynchronous rolling on the pure copper plate with the thickness of 6mm obtained in the step (1) at room temperature to obtain the copper plate with the total deformation of 33%, wherein the speed ratio of the upper roller to the lower roller in the rolling process is 1.3.
(3) And (3) annealing the pure copper plate subjected to asynchronous rolling for 15min at 450 ℃ and polishing the surface and removing the soil.
The pure copper obtained in examples and comparative examples was subjected to performance test, and the results are shown in fig. 1 (the annealed state in fig. 1 is the pure copper coarse-grain sample performance), and it can be seen from fig. 1:
in the embodiment 1, the grain double-peak and gradient structure composite isomerism pure copper obtained by surface nanocrystallization after annealing for 15min at 450 ℃ has higher yield strength and ultimate tensile strength, meanwhile, good plasticity is maintained, the yield strength and ultimate tensile strength respectively reach 192MPa and 239MPa, and the uniform elongation reaches 28%.
In comparative example 1, the grain size gradient structure prepared by surface nanocrystallization after annealing at 700 ℃ for 2 hours has improved yield strength and ultimate tensile strength of pure copper, and good plasticity is maintained; the yield strength and the ultimate tensile strength of the alloy reach 150MPa and 208MPa respectively, the uniform elongation reaches 27%, and the effect is still not good in example 1.
In comparative example 2, after annealing at 350 ℃ for 30min, the pure copper with the grain size heterostructure obtained by surface nanocrystallization has higher yield strength and ultimate tensile strength, but the plasticity of the pure copper is reduced, the yield strength and ultimate tensile strength respectively reach 206MPa and 257MPa, and the uniform elongation rate reaches 19.7%.
Comparison of example 1 with comparative example 3 shows that: comparative example 3 has higher yield strength but poorer plasticity because the copper plate of the example after being rolled and annealed for a short time has a unique grain bimodal structure, and improves the plasticity of the material. Comparison of example 1 with comparative example 4 shows that: the yield strength of comparative example 4 is far lower than that of the examples because the polished pure copper plate is subjected to surface treatment by adopting a high-energy shot blasting technology, so that the microstructure density of the polished pure copper plate has a gradual trend from the surface to the core, and the gradient structure can effectively improve the strain hardening capacity of the material, thereby improving the material strength.
The invention successfully prepares the composite isomerism pure copper which has the characteristics of a grain bimodal structure and a gradient structure. In the mechanical tensile test, the synergistic effect among the bimodal hard region and the soft region, the surface tissue and the core tissue and the combination of various deformation mechanisms jointly improve the mechanical properties of pure copper. Specifically, the yield strength is improved by a factor of 2 while maintaining good plasticity.
Claims (2)
1. A preparation method of composite isomerism pure copper with a grain double peak and gradient structure is characterized by comprising the following steps: the specific steps are as follows:
(1) Commercial oxygen-free pure copper plates with the thickness of 6mm are purchased, and the surfaces are polished to remove an oxide layer;
(2) Asynchronously rolling the pure copper plate with the thickness of 6mm obtained in the step (1) to 4mm in 3-5 times at room temperature, wherein the total deformation is 33%, and the speed ratio of the upper roller to the lower roller in the rolling process is 1.3;
(3) Annealing the rolled pure copper plate at 450 ℃ for 15min to obtain a grain bimodal structure, and polishing the surface, and removing dirt for later use;
(4) And (3) carrying out surface nanocrystallization treatment on the pure copper substrate obtained in the step (3) in a room temperature environment, and finally obtaining the pure copper with double-peak crystal grain and composite isomerism of the gradient structure.
2. The method for preparing the grain bimodal and gradient structured composite isomerism pure copper, which is characterized in that: in the step (3), the surface nanocrystallization treatment is to treat the surface by adopting a high-energy shot blasting technology, wherein the treatment time is 2min, the shot blasting rate is selected to be 30m/s, and the diameter of the steel ball is 8mm.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202410083901.5A CN117702022A (en) | 2024-01-19 | 2024-01-19 | Preparation method of composite isomerism pure copper with grain double peak and gradient structure |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202410083901.5A CN117702022A (en) | 2024-01-19 | 2024-01-19 | Preparation method of composite isomerism pure copper with grain double peak and gradient structure |
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| Publication Number | Publication Date |
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| CN117702022A true CN117702022A (en) | 2024-03-15 |
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| Application Number | Title | Priority Date | Filing Date |
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| CN202410083901.5A Pending CN117702022A (en) | 2024-01-19 | 2024-01-19 | Preparation method of composite isomerism pure copper with grain double peak and gradient structure |
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| Country | Link |
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| CN (1) | CN117702022A (en) |
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- 2024-01-19 CN CN202410083901.5A patent/CN117702022A/en active Pending
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