CN110846533A - Preparation method of Cu-Ni-Si alloy thin strip based on sub-rapid solidification - Google Patents
Preparation method of Cu-Ni-Si alloy thin strip based on sub-rapid solidification Download PDFInfo
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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
- C22C9/06—Alloys based on copper with nickel or cobalt as the next major constituent
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- B22—CASTING; POWDER METALLURGY
- B22D—CASTING OF METALS; CASTING OF OTHER SUBSTANCES BY THE SAME PROCESSES OR DEVICES
- B22D11/00—Continuous casting of metals, i.e. casting in indefinite lengths
- B22D11/06—Continuous casting of metals, i.e. casting in indefinite lengths into moulds with travelling walls, e.g. with rolls, plates, belts, caterpillars
- B22D11/0622—Continuous casting of metals, i.e. casting in indefinite lengths into moulds with travelling walls, e.g. with rolls, plates, belts, caterpillars formed by two casting wheels
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- 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
- C22F1/002—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working by rapid cooling or quenching; cooling agents used therefor
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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 relates to a preparation method of a Cu-Ni-Si alloy ribbon based on sub-rapid solidification, which comprises the following steps: smelting a Cu-Ni-Si alloy melt according to the design components, pouring into a tundish, controlling the superheat degree, pouring into a double-roller thin strip casting and rolling machine through the tundish for continuous casting, cooling the cast strip after the cast strip is taken out of a roller to prepare a cast strip with the thickness of 0.5-5.0 mm, carrying out multi-pass cold rolling after short-time solid solution to obtain a cold-rolled thin strip, and carrying out aging treatment to obtain the alloy thin strip. Because the near-net-shape thin strip can be directly formed by the molten metal, the method can save the processes of homogenizing annealing hot rolling and the like in the traditional process, shorten the flow, quickly solidify and refine the initial solidification structure of the cast strip, promote the grain boundary to tend to the development of a special sigma 3 large-angle grain boundary, simultaneously improve the supersaturation solid solubility of Si in a Cu matrix, effectively inhibit the segregation of Ni and Si, simultaneously improve the tensile strength of the aged strip to be more than or equal to 700MPa and the electric conductivity to be more than or equal to 25% IACS, and finally obtain the thin strip with excellent comprehensive performance on the basis of saving energy, reducing emission, simplifying the process and reducing.
Description
The technical field is as follows:
the invention belongs to the technical field of metallurgy, and particularly relates to a preparation method of a Cu-Ni-Si alloy thin strip based on sub-rapid solidification.
Background art:
with the development of communication, electronics and power industries, the demand for the quantity of copper alloy strips is increased sharply, and a series of new requirements on high precision, high surface, high performance and the like are provided in the aspect of product quality, but from the production condition of domestic strips, a considerable quantity of copper strip products belong to middle and low grade products, most of lead frame copper strips, transformer strips, white copper strips and the like in high-precision strips depend on import, the high-precision strip production in China is developed, and the improvement of the product quality level becomes an important task of people at present.
The Cu-Ni-Si alloy belongs to a typical aging strengthening type high-strength conductive copper alloy, has excellent performances of high strength, good conductivity, heat-resistant stability, easy processing and the like, and is widely applied to the fields of electronic connectors, lead frame materials, electronic packaging materials and the like. However, there are still many problems in the preparation process: mainly, in the traditional hot rolling process, the cooling rate of an alloy solidification structure is slow, so that the crystal grains of an initial solidification structure are coarse and have serious microsegregation, and long-term homogenization treatment is needed, a metallographic picture of an ingot solidification structure in the conventional process is shown in a figure 1(a), a metallographic picture of a casting strip solidification structure is shown in a figure 1(b), and a distribution diagram of the segregation condition of the ingot casting structure is shown in a figure 2. Therefore, a copper blank preparation process method which can realize continuous improvement of cooling rate, optimizes the traditional hot rolling process and facilitates subsequent cold rolling processing becomes the target of development at present.
The prior art discloses the preparation of Cu-Ni-Si based copper alloy, wherein when the X-ray diffraction intensity from the {111} plane in the rolled surface is I {111}, the X-ray diffraction intensity from the {111} plane in the pure copper powder standard sample is I0{111}, I {111}/I0{111} is 0.15 or more, when the X-ray diffraction intensity from the {200} plane in the rolled surface is I {200}, the X-ray diffraction intensity from the {200} plane in the pure copper powder standard sample is I0{200}, I {200}/I0{200} is 0.5 or less, when the X-ray diffraction intensity from the {220} plane in the rolled surface is I {220}, the X-ray diffraction intensity from the {311} plane is I {311}, I {111}/(I {111 + I {200 {311 + I {220} plane in the rolled surface is 0.2 or more, and the rolling coefficient is 130GPa or more, the yield strength YS in the right-angle rolling direction meets the following formula: YS ≧ 22 × (Ni mass%) 2+215 × (Ni mass%) +422, conductivity in the direction perpendicular to rolling of 30% IACS or more, and the like.
Among the numerous copper and copper alloy work materials, sheet and strip are of great importance. Is widely applied to various departments of national economy. Particularly, with the development of the electronic information industry, the demand on the quantity of copper and copper alloy strips is increased sharply, a series of new high-standard requirements are provided on the aspect of product quality, the rapid development of the copper strip production technology is promoted, the new concept of the high-precision copper strip is provided, and the brand-new high-precision copper strip production technology and method appear. Its advantages are high modernization and automation of production, and high quality of product. The traditional block production method is completely replaced by the belt production method. The production of the plate strip becomes the final process of strip production, and in production statistics, high-precision plate strip products can replace two varieties of plates and strips. In order to continuously improve the yield, reduce the cost, increase the yield and ensure the high automation of the production process, the quality of coils in the production of high-precision plate and strip materials is continuously increased, the scale of production enterprises is continuously enlarged, the management level of the enterprises is continuously improved, and the production of the high-precision plate and strip materials becomes an important component of the modern process. The development of the production technology thereof pushes the power copper processing technology to continuously move towards more modernization, and a plurality of new processing methods are continuously appeared.
In the prior art, the preparation of the Cu-Ni copper alloy needs complicated homogenization, hot rolling and other processes, and the problems of easy occurrence of segregation and the like are solved.
The invention content is as follows:
the invention aims to overcome the defects in the prior art and provide a preparation method of a Cu-Ni-Si alloy thin strip based on sub-rapid solidification, which utilizes the sub-rapid solidification characteristic and the short-flow advantage of a thin strip casting and rolling technology to cast and roll a thin strip with the thickness of 0.5-5.0 mm, omits fussy homogenization, hot rolling and other flows, improves the solid solution efficiency, refines the structure of the alloy cast strip, inhibits micro segregation and further improves the comprehensive performance.
In order to achieve the purpose, the invention adopts the following technical scheme:
a preparation method of a Cu-Ni-Si alloy thin strip based on sub-rapid solidification comprises the following steps:
(1) smelting copper alloy according to the designed components to obtain a copper alloy melt, wherein the copper alloy melt comprises 1.0-7.5% of Nis, 0.25-1.30% of Si, less than or equal to 0.05% of impurities and the balance of Cu in percentage by mass;
(2) feeding a copper alloy melt into a tundish through a pouring gate, controlling the pouring superheat degree to be 20-100 ℃ and the preheating temperature of the tundish to be 1100-1200 ℃, then pouring into a double-roller thin strip casting mill for continuous casting to prepare a casting strip with the thickness of 0.5-5.0 mm, and spraying water for quenching and cooling after the casting strip is taken out of a casting roller;
(3) carrying out solution treatment on the cast strip at 850-900 ℃ for x (0.5-1) h, polishing the surface of the cast strip subjected to solution treatment, and carrying out single-stage cold rolling to obtain a cold-rolled strip, wherein the pass reduction rate of the cold rolling is 15-20%, and the total reduction rate is 85-95%;
(4) and (3) carrying out aging treatment on the cold-rolled strip at 400-500 ℃ for 2-4 h to obtain the Cu-Ni-Si alloy thin strip.
In the step (2), the liquid level is controlled to be 50-90 mm during continuous casting, and the rotating speed of the continuous casting rod is controlled to be 35-45 m/min.
In the step (2), the solidification rate of the continuous casting process reaches 103The temperature is higher than DEG C/s;
in the step (2), the cooling mode of the cast strip is quenching cooling, and the cooling rate is 60-80 ℃/s.
In the step (4), the thickness of the Cu-Ni-Si alloy thin strip is 0.025-0.75 mm.
In the step (4), the CSL crystal boundary proportion of the prepared Cu-Ni-Si alloy thin strip solidification structure is 1.5-3%.
In the step (4), the tensile strength of the prepared Cu-Ni-Si alloy ribbon is 700-850 MPa, the conductivity of the Cu-Ni-Si alloy ribbon is 26-43.5% IACS, and the hardness of the Cu-Ni-Si alloy ribbon is 218-287 HV.
On the basis of fully utilizing the sub-rapid solidification characteristic of a twin-roll thin strip casting and rolling technology, the invention provides more definite technological parameters for obtaining the high-performance cast and rolled copper strip, such as required core technological parameters of superheat degree, liquid level height, casting and rolling speed and the like, and key technological parameters of matching of cooling speed after casting and a cooling mode and the like.
The invention has the beneficial effects that:
(1) based on the short flow advantage and the sub-rapid solidification characteristic of the twin-roll thin strip casting and rolling technology, the supersaturation solid solubility of Ni and Si elements can be effectively improved, uniform and fine solidification structures are obtained, and the grain boundary is promoted to tend to develop towards the special sigma 3 large-angle grain boundary with smaller influence on the conductivity in the casting and rolling process; the homogenizing annealing and hot rolling process in the traditional process can be omitted, the solid solution efficiency is improved, the process is simplified, the cost is reduced, and the resources are saved;
(2) the control range of casting and rolling technological parameters such as superheat degree, liquid level height, casting and rolling speed and cooling mode after casting are provided clearly, and the links are controlled properly to obtain good service performance;
(3) on the basis of a large number of scientific experiments, the CSL crystal boundary proportion of a casting strip solidification structure is improved;
(4) by adopting the thin strip continuous casting process, the cast strip with the thickness of 0.5-5.0 mm can be directly produced, a hot rolling process is omitted, the cold rolling preparation is directly carried out, and the yield is improved.
Description of the drawings:
FIG. 1 is a metallographic picture (a) of a cast ingot solidification structure and a metallographic picture (b) of a cast strip solidification structure in a conventional process;
FIG. 2 is a distribution diagram of segregation of the structure of an ingot in the conventional process;
FIG. 3 is a graph showing the structure segregation of the cast strip in example 1 of the present invention;
FIG. 4 is a distribution diagram of the structure segregation of the cast strip after 0.5h of solution treatment at 900 ℃ in example 1 of the present invention;
FIG. 5 is a distribution diagram of grain boundaries of a solidified structure of the cast strip in example 1 of the present invention;
FIG. 6 is a drawing graph of a thin strip of Cu-Ni-Si alloy prepared in example 1;
FIG. 7 is a metallographic picture of a cold-rolled thin strip in example 2 after aging treatment at 450 ℃ for 2 hours;
FIG. 8 is a metallographic picture of a cold-rolled thin strip in example 3 after being subjected to aging treatment at 500 ℃ for 3 hours;
FIG. 9 is a drawing graph of a thin strip of Cu-Ni-Si alloy prepared in example 4.
The specific implementation mode is as follows:
the present invention will be described in further detail with reference to examples.
The standard adopted by the hardness test in the embodiment of the invention is GB/T4342-1991 method for testing the metal micro Vickers hardness.
The standard adopted by the conductivity test in the embodiment of the invention is GB/T32791-2016 copper and copper alloy conductivity eddy current test method.
In the embodiment of the invention, the solidified structure of the casting strip is fine and uniform in crystal grain, and the CSL crystal boundary of the solidified structure is 1.5-3%.
In the embodiment of the invention, the pouring temperature is strictly controlled to be 1100-1200 ℃ during pouring, and water cooling is carried out immediately after the casting strip is formed.
Example 1
Smelting a Cu-Ni-Si alloy melt according to the designed components, wherein the components comprise 3.2% of Ni, 0.75% of Si, less than or equal to 0.05% of impurities and the balance of Cu in percentage by mass;
feeding a molten Cu-Ni-Si alloy melt into a tundish through a pouring gate, controlling the superheat degree to be 55 ℃ and the preheating temperature of the tundish to be 1100 ℃, pouring the molten Cu-Ni-Si alloy melt into a double-roller thin strip casting and rolling machine through the tundish for continuous casting to obtain a casting strip with the thickness of 3.0mm, wherein the solidification rate in the continuous casting process reaches 1100 ℃/s, the casting strip is immediately cooled by water spraying after being taken out of a casting roller, and the cooling speed of the casting strip is controlled to be 70 ℃/s; controlling the liquid level to be 60mm and the roller rotating speed to be 40m/min in the continuous casting process; the distribution diagram (electronic probe) of the segregation condition of the casting belt structure is shown in FIG. 3, the distribution diagram of the grain boundary of the solidification structure of the casting belt is shown in FIG. 5, and it can be seen from the diagram that the grain boundary in the casting belt structure has slight element enrichment, has typical columnar crystal and a central equiaxed crystal area, and the trend is much weaker than that of a common ingot; after cooling, the casting belt is subjected to solid solution for 0.5h at 900 ℃, and the distribution diagram of the structure segregation after solid solution is shown in FIG. 4; therefore, element enrichment, columnar crystals and the like are easy to eliminate in the subsequent heat treatment of solid solution for 0.5h at 900 ℃; the distribution of Ni and Si is relatively uniform, and the homogenization annealing and hot rolling process in the conventional hot rolling process can be omitted; the solidification structure CSL grain boundary of the cast strip was 2.95%.
After the surface of the cast strip is polished, the cast strip after the solution treatment is subjected to multi-pass cold rolling, the pass reduction rate is 15%, the total reduction rate is 90%, and a cold-rolled thin strip with the thickness of 0.3mm is obtained;
and (3) aging the cold-rolled thin strip at 450 ℃, cutting for 4h according to the size to obtain a Cu-Ni-Si alloy thin strip, wherein a drawing curve chart is shown in figure 6, and the Cu-Ni-Si alloy thin strip has the tensile strength of 721MPa, the electric conductivity of 43.5 percent IACS and the hardness of 222 HV.
Example 2
The method is the same as example 1, except that:
(1) the Cu-Ni-Si alloy melt comprises 2.5 percent of Ni and 0.5 percent of Si according to mass percent;
(2) controlling the superheat degree to be 85 ℃, the preheating temperature of the tundish to be 1150 ℃, the thickness of the casting strip to be 2.0mm, and the cooling speed of the casting strip after the casting strip is taken out of the casting roll to be 75 ℃/s; in the continuous casting process, the liquid level is controlled to be 70mm, the rotating speed of a roller is controlled to be 45m/min, and the CSL crystal boundary of a solidification structure of a cast strip is 1.93 percent;
(3) the total reduction rate of cold rolling is 90 percent; the thickness of the cold-rolled thin strip is 0.2 mm;
(4) the aging treatment temperature is 450 ℃, the time is 2h, the metallographic picture after the aging treatment is shown in figure 7, the tensile strength of the Cu-Ni-Si alloy thin strip is 750MPa, the electric conductivity is 33 percent IACS, and the hardness is 230 HV.
Example 3
The method is the same as example 1, except that:
(1) the Cu-Ni-Si alloy melt comprises 3.0 percent of Ni and 0.6 percent of Si according to mass percent;
(2) controlling the superheat degree to be 95 ℃, the preheating temperature of the tundish to be 1200 ℃, the thickness of the cast strip to be 4.0mm, and the cooling speed of the cast strip after the cast strip is taken out of the casting roll to be 75 ℃/s; in the continuous casting process, the liquid level is controlled to be 90mm, the rotating speed of a roller is controlled to be 40m/min, and the CSL crystal boundary of a solidification structure of a cast strip is 2.31 percent;
(3) the total reduction rate of cold rolling is 95 percent; the thickness of the cold-rolled thin strip is 0.2 mm;
(4) the aging treatment temperature is 500 ℃, the time is 3h, the metallographic picture after the aging treatment is shown in figure 8, the tensile strength of the Cu-Ni-Si alloy thin strip is 700MPa, the electric conductivity is 35 percent IACS, and the hardness is 218 HV.
Example 4
The method is the same as example 1, except that:
(1) the Cu-Ni-Si alloy melt comprises 6.0 percent of Ni and 1.0 percent of Si according to mass percent;
(2) controlling the superheat degree to be 65 ℃, the preheating temperature of the tundish to be 1150 ℃, the thickness of the casting strip to be 3.0mm, and the cooling speed of the casting strip after the casting strip is taken out of the casting roll to be 80 ℃/s; in the continuous casting process, the liquid level is controlled to be 50mm, the rotating speed of a roller is controlled to be 35m/min, and the CSL crystal boundary of a solidification structure of a cast strip is 1.65%;
(3) the total reduction rate of cold rolling is 90 percent; the thickness of the cold-rolled thin strip is 0.3 mm;
(4) the aging treatment temperature is 400 ℃, the time is 3h, the drawing curve chart of the Cu-Ni-Si alloy thin strip is shown in figure 9, the tensile strength is 850MPa, the electric conductivity is 26 percent IACS, and the hardness is 287 HV.
Claims (7)
1. A preparation method of a Cu-Ni-Si alloy thin strip based on sub-rapid solidification is characterized by comprising the following steps:
(1) smelting copper alloy according to the designed components to obtain a copper alloy melt, wherein the copper alloy melt comprises 1.0-7.5% of Nis, 0.25-1.30% of Si, less than or equal to 0.05% of impurities and the balance of Cu in percentage by mass;
(2) feeding a copper alloy melt into a tundish through a pouring gate, controlling the pouring superheat degree to be 20-100 ℃ and the preheating temperature of the tundish to be 1100-1200 ℃, then pouring into a double-roller thin strip casting mill for continuous casting to prepare a casting strip with the thickness of 0.5-5.0 mm, and spraying water for quenching and cooling after the casting strip is taken out of a casting roller;
(3) carrying out solution treatment on the cast strip at 850-900 ℃ for x (0.5-1) h, polishing the surface of the cast strip subjected to solution treatment, and carrying out single-stage cold rolling to obtain a cold-rolled strip, wherein the pass reduction rate of the cold rolling is 15-20%, and the total reduction rate is 85-95%;
(4) and (3) carrying out aging treatment on the cold-rolled strip at 400-500 ℃ for 2-4 h to obtain the Cu-Ni-Si alloy thin strip.
2. The method for preparing the Cu-Ni-Si alloy ribbon based on the sub-rapid solidification according to the claim 1, wherein in the step (2), the liquid level height is controlled to be 50-90 mm during continuous casting, and the rotating speed of a continuous casting rod is controlled to be 35-45 m/min.
3. The method for preparing the Cu-Ni-Si alloy ribbon based on the sub-rapid solidification according to the claim 1, wherein in the step (2), the solidification rate of the continuous casting process reaches 103The temperature is higher than the second temperature.
4. The method for preparing the Cu-Ni-Si alloy ribbon based on the sub-rapid solidification according to the claim 1, wherein in the step (2), the cooling mode of the cast ribbon is quenching cooling, and the cooling rate is 60-80 ℃/s.
5. The method for preparing the Cu-Ni-Si alloy ribbon based on the sub-rapid solidification according to the claim 1, wherein in the step (4), the thickness of the Cu-Ni-Si alloy ribbon is 0.025-0.75 mm.
6. The method for preparing the Cu-Ni-Si alloy ribbon based on the sub-rapid solidification according to the claim 1, wherein the CSL grain boundary proportion of the solidification structure of the prepared Cu-Ni-Si alloy ribbon in the step (4) is 1.5-3%.
7. The method for preparing the Cu-Ni-Si alloy ribbon based on the sub-rapid solidification according to the claim 1, wherein the tensile strength of the prepared Cu-Ni-Si alloy ribbon in the step (4) is 700-850 MPa, the electric conductivity is 26-43.5% IACS, and the hardness is 218-187 HV.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN111155020A (en) * | 2020-01-20 | 2020-05-15 | 东南大学 | Method for regulating and controlling corrosion resistance of CoNiFe intermediate entropy alloy |
| CN114752810A (en) * | 2022-03-24 | 2022-07-15 | 江苏恒盈电子科技有限公司 | High-strength semiconductor lead frame for circuit board and preparation method thereof |
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| CN108359836A (en) * | 2018-03-12 | 2018-08-03 | 东北大学 | A kind of preparation method of the Cu-Cr-Zr alloy thin bands based on Sub realizable fuzzy matrix |
| CN108453222A (en) * | 2018-03-12 | 2018-08-28 | 东北大学 | A kind of minimizing preparation method of Copper-Nickel-Aluminium Alloy strip |
| CN109504873A (en) * | 2017-09-14 | 2019-03-22 | 捷客斯金属株式会社 | The excellent Cu-Ni-Si series copper alloy of die wear |
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| CN101270423A (en) * | 2007-03-19 | 2008-09-24 | 日矿金属加工株式会社 | Cu-Ni-Si based copper alloy for electronic material |
| CN109504873A (en) * | 2017-09-14 | 2019-03-22 | 捷客斯金属株式会社 | The excellent Cu-Ni-Si series copper alloy of die wear |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN111155020A (en) * | 2020-01-20 | 2020-05-15 | 东南大学 | Method for regulating and controlling corrosion resistance of CoNiFe intermediate entropy alloy |
| CN114752810A (en) * | 2022-03-24 | 2022-07-15 | 江苏恒盈电子科技有限公司 | High-strength semiconductor lead frame for circuit board and preparation method thereof |
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Application publication date: 20200228 |