CN115386766A - Cu-Ni-Si-Cr-Mg quinary copper alloy and preparation method thereof - Google Patents
Cu-Ni-Si-Cr-Mg quinary copper alloy and preparation method thereof Download PDFInfo
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- C22C9/00—Alloys based on copper
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- 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
Abstract
The invention belongs to the technical field of materials and preparation and processing, and particularly relates to a Cu-Ni-Si-Cr-Mg quinary copper alloy and a preparation method thereof. The alloy comprises the following components in percentage by mass: 2.8 to 3.2 percent of Ni, 0.6 to 0.8 percent of Si, 0.05 to 0.6 percent of Cr, 0.04 to 0.1 percent of Mg and the balance of Cu. The alloy can be prepared by two short-process preparation methods: (1) Vacuum induction melting and casting → homogenization treatment → hot forging → double milling face → hot rolling → solid solution → cold rough rolling → primary aging → cold finish rolling → secondary aging; (2) Down-drawing continuous casting → continuous extrusion of bar → cold rough rolling → primary aging → cold finish rolling → secondary aging. The Cu-Ni-Si-Cr-Mg alloy has the advantages of high hardness, high conductivity, low production cost and the like, and meets the use requirements of large-scale and ultra-large-scale integrated circuit lead frames and high-end electronic element connector copper alloys.
Description
Technical Field
The invention belongs to the technical field of materials and preparation and processing, and particularly relates to a Cu-Ni-Si-Cr-Mg quinary copper alloy and a preparation method thereof.
Background
Electronic technology is one of important forces for modern scientific and technical development, has the characteristics of strategic, basic and precedent and the like, and is closely connected with national defense construction and national economy development. With the rapid advance of large-scale and ultra-large-scale integrated circuits, the lead frame is used as a framework of the integrated circuit and a bridge for connecting a semiconductor chip with an external circuit, and the material of the lead frame has the characteristics of high strength and high conductivity. The electronic component connector serves as a core component of the electric connector and mainly plays roles in energy transmission and information exchange, the application field is very wide and almost covers all scenes of optical and electric signal transmission interaction, and the high-end electronic component connector has stricter requirements on materials. Copper alloy has good electrical conductivity and thermal conductivity, strong tensile strength and hardness, and good plastic processability, and gradually becomes the main material of lead frames and electronic component connectors, while Cu-Ni-Si alloy is increasingly favored by domestic and foreign scholars due to excellent service performance and low industrial production cost. For example:
the patent application: the lead frame copper alloy with easy smelting, composite precipitation strengthening, high tensile strength and high conductivity is prepared by a fusion casting → homogenization → hot rolling → double-sided milling → rough cold rolling → trimming → primary online quenching → pre-finish rolling → secondary online quenching → primary finish rolling → primary aging → secondary finish rolling → secondary aging preparation method.
The patent application: a processing technology (publication No. CN 107988512A) of a high-strength high-elasticity copper-nickel-silicon-cobalt lead frame is provided, aiming at a large-scale and super-large-scale lead frame and a precise plug-in terminal Cu-Ni-Si copper alloy, co, mg, rare earth elements and other metal elements are added, and a strip with the yield strength of 800-850 MPa and the electric conductivity of more than or equal to 45% is obtained by utilizing a smelting → heating → hot rolling → solid solution → face milling → primary rolling → primary annealing → intermediate rolling → secondary annealing → finish rolling → aging processing technology.
The patent application: "Cu-Ni-Si-Mg based alloy (publication No. CN 102105611A) with improved conductivity and bendability" has been proposed to add Mg element to a Cu-Ni-Si based copper alloy, which can maintain high strength, high conductivity and good bending workability.
The patent application: "Cu-Ni-Si-Co-Cr alloy for electronic materials (publication No. CN 101983249A)", it is proposed that a copper alloy for electronic materials having high strength and high conductivity is obtained by adding Co and Cr elements to a Cu-Ni-Si based alloy. The patent application: "Cu-Ni-Si based alloy for electronic materials (publication No. CN 101270423A)", a Cu-Ni-Si-Cr based copper alloy was proposed, and a copper alloy for electronic materials having excellent properties was obtained in the same manner.
Although the above researches have obtained the lead frame and the electronic connector copper alloy material with better performance by adding alloy strengthening elements and corresponding preparation means, the complex alloy system and the lengthy preparation process make industrial production cost and the environmental protection concept of energy conservation and emission reduction increasingly emphasized along with the development of electronic technology.
Disclosure of Invention
In view of the above, the present invention provides a Cu-Ni-Si-Cr-Mg quinary copper alloy and a preparation method thereof, which can optimize alloy strengthening elements, shorten process flow, and realize low-cost, low-energy consumption, low-emission, high-performance and short-flow preparation of lead frame and electronic component connector copper alloy under the condition of ensuring that the copper alloy meets the requirements of high strength and high conductivity of large-scale and ultra-large-scale lead frame and high-end electronic component connector copper alloy.
In order to achieve the purpose, the technical scheme of the invention is as follows:
the Cu-Ni-Si-Cr-Mg quinary copper alloy comprises the following components in percentage by mass: 2.8 to 3.2 percent of Ni, 0.6 to 0.8 percent of Si, 0.05 to 0.6 percent of Cr, 0.04 to 0.1 percent of Mg and the balance of Cu.
The Cu-Ni-Si-Cr-Mg quinary copper alloy comprises the following alloy components in percentage by mass: 2.95 to 3.05 percent of Ni, 0.65 to 0.7 percent of Si, 0.07 to 0.1 percent of Mg, 0.07 to 0.1 percent of Cr or 0.4 to 0.5 percent of Cr according to the using requirement, and the balance of Cu.
The preparation method of the Cu-Ni-Si-Cr-Mg quinary copper alloy comprises the following steps:
(1) Vacuum induction casting;
(2) Homogenizing;
(3) Hot forging;
(4) Double milling surfaces;
(5) Hot rolling;
(6) Solid solution;
(7) Cold rough rolling: the single-pass deformation of the cold rough rolling is 15-30%, the total deformation of the cold rough rolling is 83-90%, and the thickness of the cold rough rolled is 0.5-1.2 mm;
(8) Primary aging: the aging temperature is 360-560 ℃, and the aging time is 0.5-16 h;
(9) Cold finish rolling: the total deformation of cold finish rolling is 40-92%, and the thickness after cold finish rolling is 0.1-0.3 mm;
(10) Secondary aging: the aging temperature is 360-560 ℃, and the aging time is 0.5-16 h.
The preparation method of the Cu-Ni-Si-Cr-Mg quinary copper alloy is characterized in that the vacuum induction casting is as follows: proportionally placing electrolytic Cu with the purity of more than 99.96wt%, electrolytic Ni with the purity of more than 99.96wt% and polycrystalline Si with the purity of more than 99.99wt% into a crucible of a vacuum induction furnace in sequence according to the principle of tightness at the bottom, vacuumizing until the air pressure is below 5Pa, starting heating for melting, after all the materials are melted, adjusting the temperature to 1185-1215 ℃, refining for 15-20 min, filling argon into the crucible after refining, adding Mg with the purity of more than 99.96wt% and Cr with the purity of more than 99.99wt% wrapped by copper foil through a secondary feeding bin, stirring uniformly after the liquid level is calm and no bubble escapes, namely complete melting, and carrying out charged casting during casting at the temperature of 1155-1165 ℃.
The preparation method of the Cu-Ni-Si-Cr-Mg quinary copper alloy is characterized by comprising the following steps of: the ingot is kept at 900-1000 ℃ for 1-5 hours.
The preparation method of the Cu-Ni-Si-Cr-Mg quinary copper alloy is characterized by comprising the following steps: the forging temperature is more than or equal to 900 ℃, the finish forging temperature is more than or equal to 700 ℃, and the forging ratio is 2.2-3.7.
The preparation method of the Cu-Ni-Si-Cr-Mg quinary copper alloy has the characteristics that: and (4) milling the two surfaces according to the requirement to remove the defects on the surface of the hot-forged plate, wherein the milling depth is 0.1-0.5 mm.
The preparation method of the Cu-Ni-Si-Cr-Mg quinary copper alloy is characterized by comprising the following steps: the initial rolling temperature is more than or equal to 850 ℃, the final rolling temperature is more than or equal to 700 ℃, the hot rolling single-pass deformation is 10-35%, the hot rolling total deformation is 70-85%, and the thickness after hot rolling is 5-8 mm.
The preparation method of the Cu-Ni-Si-Cr-Mg quinary copper alloy has the solid solution characteristics that: the solid solution temperature is 800-1000 ℃, and the solid solution time is 1-5 h.
The preparation method of the Cu-Ni-Si-Cr-Mg quinary copper alloy comprises the following steps:
(1) Downward-drawing continuous casting;
(2) Continuously extruding the bar;
(3) Cold rough rolling: the single-pass deformation of the cold rough rolling is 15-30%, the total deformation of the cold rough rolling is 83-90%, and the thickness after the cold rough rolling is 0.5-1.2 mm;
(4) Primary aging: the aging temperature is 360-560 ℃, and the aging time is 0.5-16 h;
(5) Cold finish rolling: the total deformation of cold finish rolling is 40-92%, and the thickness after cold finish rolling is 0.1-0.3 mm;
(6) Secondary aging: the aging temperature is 360-560 ℃, and the aging time is 0.5-16 h.
The design idea of the invention is as follows:
based on a Cu-Ni-Si alloy system, different types of strengthening phases are precipitated by adding alloy elements on the basis of the original precipitation of a single phase by utilizing the characteristic of precipitation of strengthening phases in the aging process, so that the dual-phase strengthening is realized, and the influence of the alloy on the reduction of the electric conductivity is realized while the strength is improved by adding Cr elements with lower solid solubility with Cu at room temperature. In order to fully realize the double-phase strengthening synergistic effect, the precipitation of a strengthening phase can be further promoted by introducing cold finish rolling and secondary aging on the preparation method, the conductivity of the alloy is improved, the dislocation strengthening effect can be enhanced by the cold finish rolling, and the strength of the copper alloy is further improved.
The invention has the advantages and beneficial effects that:
1. the invention can optimize alloy strengthening elements, shorten process flow and realize the low-cost, low-energy consumption, low-emission, high-performance and short-flow preparation of the lead frame and the copper alloy of the connector of the electronic component device under the condition of ensuring that the requirements of high strength and high conductivity of the copper alloy of the lead frame and the connector of the high-end electronic component device on large scale and super large scale are met.
2. Ni formation during the secondary aging treatment of the invention 2 Si phase and Cr phase 3 The Si phase enables the alloy to generate a dual-phase strengthening effect, and simultaneously Ni, si and Cr elements which are dissolved in the Cu matrix are precipitated and separated out, so that the conductivity of the alloy is improved. The thickness of the strip after the cold finish rolling is 0.1 to 0.3mm, the tensile strength of the alloy in the secondary peak aging state is more than 830MPa, and the electric conductivity is more than 40 percent IACS.
Drawings
FIG. 1 is a flow chart of a first preparation method of a Cu-Ni-Si-Cr-Mg quinary copper alloy.
FIG. 2 is a flow chart of a second preparation method of a Cu-Ni-Si-Cr-Mg quinary copper alloy.
Detailed Description
In the specific implementation process, the Cu-Ni-Si-Cr-Mg quinary copper alloy can be prepared by two short-flow preparation methods, and the specific flow is as follows: (1) Vacuum induction melting and casting → homogenization treatment → hot forging → double milling face → hot rolling → solid solution → cold rough rolling → primary aging → cold finish rolling → secondary aging; (2) Down-drawing continuous casting → continuous extrusion of bar → cold rough rolling → primary aging → cold finish rolling → secondary aging.
Hereinafter, embodiments of the present invention will be described in further detail with reference to the drawings.
Example 1:
the embodiment designs and develops a quinary copper alloy which meets the requirements of high strength and high conductivity of large-scale and ultra-large-scale lead frames and high-end electronic component connectors: cu-3.03Ni-0.69Si-0.074Cr-0.081Mg (wt.%), and the strengthening phase of the copper alloy is Ni 2 Si phase and Cr phase 3 A Si phase.
As shown in FIG. 1, the preparation method of the Cu-Ni-Si-Cr-Mg quinary alloy is specifically described as follows:
(1) Vacuum induction fusion casting: proportionally placing electrolytic Cu with the purity of more than 99.96wt%, electrolytic Ni with the purity of more than 99.96wt% and polycrystalline Si with the purity of more than 99.99wt% into a crucible of a vacuum induction furnace in sequence according to the principle of tightness at the bottom, vacuumizing until the air pressure is 4Pa, starting to heat up, adjusting the temperature to 1215 ℃ after the materials are all melted, refining for 15min, filling argon into the crucible after refining, putting Mg with the purity of more than 99.96wt% and Cr with the purity of more than 99.99wt% into the crucible through a secondary feeding bin, and stirring uniformly after the liquid level is calm and no bubble escapes, namely completely melting down, carrying out charged casting during casting, and controlling the temperature at 1165 ℃.
(2) Homogenizing: the ingot was held at 960 ℃ for 2h.
(3) Hot forging: the open forging temperature is 960 ℃, the finish forging temperature is 780 ℃, and the forging ratio is 2.4.
(4) Double milling: and removing the defects on the surface of the hot-forged plate, and milling to a depth of 0.2mm.
(5) Hot rolling: the initial rolling temperature is 900 ℃, the final rolling temperature is 750 ℃, the rolling is carried out for 6 times, the hot rolling single-pass deformation is respectively 13.3%, 19.2%, 21.4%, 24.2%, 32% and 29.4%, the hot rolling total deformation is 80% (the single-pass deformation is the ratio of the single-pass deformation value of each pass to the last thickness, the total deformation is the ratio of the total deformation value to the original hot rolling thickness, the same applies below), and the thickness after the hot rolling is 6mm.
(6) Solid solution: the solid solution temperature is 860 ℃, and the solid solution time is 1h.
(7) Cold rough rolling: the total number of the cold rough rolling passes is 7, the single-pass deformation of the cold rough rolling passes is 25%, 20%, 19.4%, 24.1%, 27.3%, 25% and 16.7%, the total deformation of the cold rough rolling passes is 83.3% (the single-pass deformation is the ratio of the single-pass deformation value of each pass to the last thickness, the total deformation is the ratio of the total deformation value to the original hot rolling thickness, the same is applied below), and the thickness after the cold rough rolling is 1mm.
(8) Primary aging: the aging temperature is 460 ℃, and the aging time is 2h.
(9) Cold finish rolling: the total deformation of the cold finish rolling is 70 percent, and the thickness of the cold finish rolling is 0.3mm.
(10) Secondary aging: the aging temperature is 410 ℃, and the aging time is 2h.
In the present example, the alloy tensile strength after aging was more than 840MPa, and the conductivity was more than 42% IACS.
Example 2:
the embodiment designs and develops a quinary copper alloy which meets the requirements of high strength and high conductivity of large-scale and ultra-large-scale lead frames and high-end electronic component connectors: cu-2.99Ni-0.67Si-0.4Cr-0.077Mg (wt%), the strengthening phase of the copper alloy is Ni 2 Si phase and Cr phase 3 A Si phase.
As shown in FIG. 1, the preparation method of the Cu-Ni-Si-Cr-Mg quinary alloy is specifically described as follows:
(1) Vacuum induction casting: proportionally placing electrolytic Cu with the purity of more than 99.96wt%, electrolytic Ni with the purity of more than 99.96wt% and polycrystalline Si with the purity of more than 99.99wt% into a crucible of a vacuum induction furnace in sequence according to the principle of tightness at the bottom, vacuumizing until the air pressure is 3Pa, starting to heat up, after all the materials are melted, adjusting the temperature to 1215 ℃, refining for 15min, filling argon into the crucible after refining, adding Mg with the purity of more than 99.96wt% and Cr with the purity of more than 99.99wt% wrapped by copper foil through a secondary feeding bin, and after the liquid level is calm and no bubbles escape, namely completely melting down, uniformly stirring, carrying out electric casting during casting, and controlling the temperature to be 1165 ℃.
(2) Homogenizing: the ingot is kept at 960 ℃ for 2h.
(3) Hot forging: the open forging temperature is 960 ℃, the finish forging temperature is 780 ℃, and the forging ratio is 2.4.
(4) Double milling: and removing the defects on the surface of the hot-forged plate, and milling to a depth of 0.2mm.
(5) Hot rolling: the initial rolling temperature is 900 ℃, the final rolling temperature is 750 ℃, the rolling is carried out for 6 times, the hot rolling single-pass deformation is respectively 13.3%, 19.2%, 21.4%, 24.2%, 32% and 29.4%, the hot rolling total deformation is 80%, and the thickness after hot rolling is 6mm.
(6) Solid solution: the solid solution temperature is 960 ℃, and the solid solution time is 1h.
(7) Cold rough rolling: the deformation of the cold rough rolling single pass is 25%, 20%, 19.4%, 24.1%, 27.3%, 25% and 16.7% in 7 passes, the total deformation of the cold rough rolling is 83.3%, and the thickness of the cold rough rolled is 1mm.
(8) Primary aging: the aging temperature is 460 ℃, and the aging time is 2h.
(9) Cold finish rolling: the total deformation of the cold finish rolling is 70 percent, and the thickness of the cold finish rolling is 0.3mm.
(10) Secondary aging: the aging temperature is 410 ℃, and the aging time is 2h.
In this example, the alloy tensile strength after aging was greater than 830MPa, the conductivity was greater than 40% IACS.
Example 3:
the embodiment designs and develops a quinary copper alloy meeting the requirements of high strength and high conductivity of large-scale and super-large-scale lead frames and high-end electronic component connectors: cu-3Ni-0.65Si-0.4Cr-0.1Mg (wt%), the strengthening phase of the copper alloy is Ni 2 Si phase and Cr phase 3 A Si phase.
As shown in FIG. 2, the preparation method of the Cu-Ni-Si-Cr-Mg quinary alloy is described as follows:
(1) And (4) downward drawing and continuous casting.
(2) And (4) continuously extruding the bar.
(3) Cold rough rolling: the deformation of the cold rough rolling single pass is 25%, 20%, 19.4%, 24.1%, 27.3%, 25% and 16.7% in 7 passes, the total deformation of the cold rough rolling is 83.3%, and the thickness of the cold rough rolled is 1mm.
(4) Primary aging: the aging temperature is 460 ℃, and the aging time is 2h.
(5) Cold finish rolling: the total deformation of the cold finish rolling is 70 percent, and the thickness of the cold finish rolling is 0.3mm.
(6) Secondary aging: the aging temperature is 410 ℃, and the aging time is 2h.
In this example, the alloy tensile strength after aging was more than 835MPa, and the electrical conductivity was more than 42% IACS.
The embodiment result shows that the Cu-Ni-Si-Cr-Mg alloy has the advantages of high hardness, high conductivity, low production cost and the like, and meets the use requirements of large-scale and ultra-large-scale integrated circuit lead frames and high-end electronic element device connector copper alloys.
The above-mentioned embodiments are only preferred embodiments of the present invention, and the scope of the present invention is not limited thereto, and any simple modifications or equivalent substitutions of the technical solutions that can be obviously obtained by those skilled in the art within the technical scope of the present invention are included in the scope of the present invention.
Claims (10)
1. The Cu-Ni-Si-Cr-Mg quinary copper alloy is characterized by comprising the following components in percentage by mass: 2.8 to 3.2 percent of Ni, 0.6 to 0.8 percent of Si, 0.05 to 0.6 percent of Cr, 0.04 to 0.1 percent of Mg and the balance of Cu.
2. The Cu-Ni-Si-Cr-Mg quinary copper alloy according to claim 1, wherein the alloy comprises the following components in percentage by mass: 2.95 to 3.05 percent of Ni, 0.65 to 0.7 percent of Si, 0.07 to 0.1 percent of Mg, 0.07 to 0.1 percent of Cr or 0.4 to 0.5 percent of Cr according to the using requirement, and the balance of Cu.
3. The method for preparing Cu-Ni-Si-Cr-Mg quinary copper alloy according to claim 1 or 2, which is characterized by comprising the following steps:
(1) Vacuum induction fusion casting;
(2) Carrying out homogenization treatment;
(3) Hot forging;
(4) Double milling surfaces;
(5) Hot rolling;
(6) Solid solution;
(7) Cold rough rolling: the single-pass deformation of the cold rough rolling is 15-30%, the total deformation of the cold rough rolling is 83-90%, and the thickness after the cold rough rolling is 0.5-1.2 mm;
(8) Primary aging: the aging temperature is 360-560 ℃, and the aging time is 0.5-16 h;
(9) Cold finish rolling: the total deformation of cold finish rolling is 40-92%, and the thickness after cold finish rolling is 0.1-0.3 mm;
(10) Secondary aging: the aging temperature is 360-560 ℃, and the aging time is 0.5-16 h.
4. The method for producing the Cu-Ni-Si-Cr-Mg quinary copper alloy according to claim 3, wherein the vacuum induction fusion casting is characterized in that: proportionally placing electrolytic Cu with the purity of more than 99.96wt%, electrolytic Ni with the purity of more than 99.96wt% and polycrystalline Si with the purity of more than 99.99wt% into a crucible of a vacuum induction furnace in sequence according to the principle of tightness at the bottom, vacuumizing until the air pressure is less than 5Pa, starting heating and melting, adjusting the temperature to 1185-1215 ℃ after the materials are all melted, refining for 15-20 min, filling argon into the crucible after refining, putting Mg with the purity of more than 99.96wt% and Cr with the purity of more than 99.99wt% wrapped by copper foil into the crucible through a secondary feeding bin, stirring uniformly after the liquid level is calm and no bubble is escaped, namely completely melting, carrying out charged casting during casting, and controlling the temperature to be 1155-1165 ℃.
5. The method for preparing Cu-Ni-Si-Cr-Mg quinary copper alloy as claimed in claim 3, wherein the homogenization treatment is characterized in that: the ingot is kept at 900-1000 ℃ for 1-5 hours.
6. The method for producing the Cu-Ni-Si-Cr-Mg quinary copper alloy as claimed in claim 3, wherein the hot forging is characterized in that: the forging temperature is more than or equal to 900 ℃, the finish forging temperature is more than or equal to 700 ℃, and the forging ratio is 2.2-3.7.
7. The method for preparing the Cu-Ni-Si-Cr-Mg quinary copper alloy according to claim 3, wherein the double milling is characterized in that: and (4) performing double-sided milling according to the requirement to remove the defects on the surface of the hot-forged plate, wherein the milling depth is 0.1-0.5 mm.
8. The method for producing the Cu-Ni-Si-Cr-Mg quinary copper alloy according to claim 3, wherein the hot rolling is characterized in that: the initial rolling temperature is more than or equal to 850 ℃, the final rolling temperature is more than or equal to 700 ℃, the hot rolling single-pass deformation is 10-35%, the hot rolling total deformation is 70-85%, and the thickness after hot rolling is 5-8 mm.
9. The method for producing the Cu-Ni-Si-Cr-Mg quinary copper alloy according to claim 3, wherein the solid solution characteristic is: the solid solution temperature is 800-1000 ℃, and the solid solution time is 1-5 h.
10. The method for preparing Cu-Ni-Si-Cr-Mg quinary copper alloy according to claim 1 or 2, which is characterized by comprising the following steps:
(1) Downward-drawing continuous casting;
(2) Continuously extruding the bar;
(3) Cold rough rolling: the single-pass deformation of the cold rough rolling is 15-30%, the total deformation of the cold rough rolling is 83-90%, and the thickness after the cold rough rolling is 0.5-1.2 mm;
(4) Primary aging: the aging temperature is 360-560 ℃, and the aging time is 0.5-16 h;
(5) Cold finish rolling: the total deformation of cold finish rolling is 40-92%, and the thickness after cold finish rolling is 0.1-0.3 mm;
(6) Secondary aging: the aging temperature is 360-560 ℃, and the aging time is 0.5-16 h.
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| CN106244849A (en) * | 2016-10-13 | 2016-12-21 | 龙岩学院 | A kind of preparation method of intensified by ultrasonic wave high property copper alloy |
| CN108193080A (en) * | 2016-12-08 | 2018-06-22 | 北京有色金属研究总院 | High intensity, highly conductive proof stress relaxation corson alloy material and preparation method thereof |
| CN108149062A (en) * | 2018-02-10 | 2018-06-12 | 中南大学 | A kind of strong high conductive copper alloy of superelevation and preparation method thereof |
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