CN116640961A - Cu-Ni-Si alloy material for lead frame and preparation method thereof - Google Patents

Cu-Ni-Si alloy material for lead frame and preparation method thereof Download PDF

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Publication number
CN116640961A
CN116640961A CN202310465955.3A CN202310465955A CN116640961A CN 116640961 A CN116640961 A CN 116640961A CN 202310465955 A CN202310465955 A CN 202310465955A CN 116640961 A CN116640961 A CN 116640961A
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rolling
cold rolling
pure
alloy
heating
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王朝辉
艾鑫宇
杜文博
李淑波
刘轲
杜宪
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Beijing University of Technology
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Beijing University of Technology
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    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C9/00Alloys based on copper
    • C22C9/06Alloys based on copper with nickel or cobalt as the next major constituent
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B21MECHANICAL METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL; PUNCHING METAL
    • B21CMANUFACTURE OF METAL SHEETS, WIRE, RODS, TUBES OR PROFILES, OTHERWISE THAN BY ROLLING; AUXILIARY OPERATIONS USED IN CONNECTION WITH METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL
    • B21C37/00Manufacture of metal sheets, bars, wire, tubes or like semi-manufactured products, not otherwise provided for; Manufacture of tubes of special shape
    • B21C37/02Manufacture of metal sheets, bars, wire, tubes or like semi-manufactured products, not otherwise provided for; Manufacture of tubes of special shape of sheets
    • CCHEMISTRY; METALLURGY
    • C21METALLURGY OF IRON
    • C21DMODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
    • C21D9/00Heat treatment, e.g. annealing, hardening, quenching or tempering, adapted for particular articles; Furnaces therefor
    • C21D9/0081Heat treatment, e.g. annealing, hardening, quenching or tempering, adapted for particular articles; Furnaces therefor for slabs; for billets
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C1/00Making non-ferrous alloys
    • C22C1/02Making non-ferrous alloys by melting
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22FCHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
    • C22F1/00Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
    • C22F1/02Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working in inert or controlled atmosphere or vacuum
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22FCHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
    • C22F1/00Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
    • C22F1/08Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working of copper or alloys based thereon
    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02EREDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E60/00Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
    • Y02E60/10Energy storage using batteries

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Mechanical Engineering (AREA)
  • Materials Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Physics & Mathematics (AREA)
  • Thermal Sciences (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Lead Frames For Integrated Circuits (AREA)
  • Conductive Materials (AREA)

Abstract

A Cu-Ni-Si alloy material for a lead frame and a preparation method thereof relate to the technical field of copper alloy processing for the lead frame. The material comprises the following components: 2.4% of Ni, 0.6% of Si, 0.2% of Mg, 0.01% of Zn, and the balance of copper and unavoidable impurities. The preparation method comprises the following steps: smelting, hot rolling, softening annealing, primary cold rolling, solid solution, secondary cold rolling, primary aging heat treatment, secondary aging heat treatment, rolling of finished products, stretch bending straightening and stress relief annealing. The book is provided withThe invention obtains Ni containing fine dispersion distribution by controlling the temperature of the secondary aging heat treatment of the strip 2 Si and Ni 3 Si 2 The microstructure of the phase effectively improves the alloy strength.

Description

Cu-Ni-Si alloy material for lead frame and preparation method thereof
Technical Field
The invention relates to the technical field of copper alloy processing for lead frames, in particular to a Cu-Ni-Si alloy material for lead frames and a preparation method thereof.
Background
The Cu-Ni-Si alloy has higher strength, better heat and electric conductivity, good processing performance and corrosion resistance, and gradually becomes an important lead frame preparation material. With the vigorous development of the electronic information industry in the current society, the development of low cost, high density, high performance and high reliability of integrated circuits has become a mainstream trend, and correspondingly, higher performance requirements are put forward on Cu-Ni-Si alloys for lead frames, besides the short-range and high-efficiency alloy preparation process, the alloys are required to have higher tensile strength and conductivity.
However, in general, there is a conflict between high strength and high conductivity, and the conductivity of the alloy is inevitably impaired while the strength of the alloy is improved. Therefore, finding a good balance between alloy strength and electrical conductivity is critical for preparing copper alloy strips for high performance lead frames. The quality of the precipitation strengthening effect of the Cu-Ni-Si alloy as a precipitation strengthening copper alloy depends on the size, distribution, number, and orientation relationship between the precipitated phases and the matrix. The method has important significance in obtaining the high-strength high-conductivity copper alloy with excellent performance by regulating and controlling the aging temperature in the two-stage aging heat treatment process.
In view of this, we have proposed the present invention.
Disclosure of Invention
Aiming at the defects and shortcomings of the prior art of lead frames, the primary purpose of the invention is to provide a Cu-Ni-Si alloy for lead frames, which aims at improving the strength and the hardness of copper alloy materials and simultaneously keeping the conductivity and the heat conductivity coefficient of the materials as much as possible, thereby meeting various requirements of the electronic industry field on the performance of the lead frame materials.
Another object of the present invention is to provide a method for producing a Cu-Ni-Si alloy for a lead frame.
It is a further object of the present invention to provide an application of a Cu-Ni-Si alloy for lead frames.
The aim of the invention is realized by the following technical scheme:
a copper alloy for a high-performance lead frame comprises the following alloy materials in percentage by mass:
2.4% of Ni, 0.6% of Si, 0.2% of Mg, 0.01% of Zn, and the balance of copper and unavoidable impurities.
The invention provides a preparation method of a copper alloy material for a high-performance lead frame, which comprises the following process flows:
smelting, hot rolling, softening annealing, primary cold rolling, solid solution, secondary cold rolling, primary aging heat treatment
The method comprises the following steps of secondary aging heat treatment, finished product rolling, stretch bending straightening, stress relief annealing:
(1) According to the content of 2.4 percent of Ni, 0.6 percent of Si, 0.2 percent of Mg and 0.01 percent of Zn, in the copper alloy composition, cu adopts electrolytic Cu, ni adopts electrolytic Ni, si adopts pure Si, mg adopts pure Mg, zn adopts pure Zn, and oxide skin on the surface is weighed and removed according to the mass percentage; the purity of the electrolytic Cu, the electrolytic Ni, the pure Si and the pure Mg and the pure Zn is over 99.9 percent.
(2) Smelting: adding the electrolytic Cu and the electrolytic Ni in the step (1) into a smelting furnace, and heating to 1300 DEG C
Melting, adding pure Si after the copper liquid is melted, fully stirring, then preserving heat for 15min, adding pure Mg and pure Zn, and pouring into ingots after stirring;
(3) And (3) hot rolling: heating the cast ingot obtained in the step (2) to 925 ℃, preserving heat for 2 hours, and then rolling, wherein the hot rolling reduction rate is 80%;
(4) Softening and annealing: immediately water-cooling the plate strip obtained in the step (3), then heating to 550 ℃ and preserving heat for 6 hours, wherein the annealing process adopts reducing gas for protection;
(5) Primary cold rolling: cold rolling the sheet material obtained in the step (4), wherein the primary cold rolling reduction is 65%;
(6) Solid solution: carrying out solid solution treatment on the plate obtained in the step (5) by adopting an air cushion annealing furnace, wherein the solid solution temperature is 970 ℃, the heat preservation time is 1h, and reducing gas is adopted for protection in the solid solution process;
(7) Secondary cold rolling: cold rolling the sheet material obtained in the step (6), wherein the secondary cold rolling reduction rate is 50%;
(8) Primary aging heat treatment: heating the plate obtained in the step (7) to 150 ℃ and preserving heat for 6 hours;
(9) And (3) secondary aging heat treatment: heating the plate obtained in step (8) to 400-550 ℃ and preserving heat for 2h (further preferably 500-550 ℃);
(10) And (3) rolling a finished product: cold rolling the sheet material obtained in the step (9), wherein the rolling reduction of the finished product is about 30%;
(11) Stretch bending and straightening: stretch bending and straightening are carried out on the plate obtained in the step (10);
(12) Stress relief annealing: heating the plate in the step (11) to 360 ℃, preserving heat for 5 hours, and naturally cooling to room temperature.
The principle and the advantages of the invention are as follows:
by controlling the content of Ni element and Si element in Cu-Ni-Si alloy and regulating and controlling the two-stage aging heat treatment process, ni with fine dispersion is fully separated out and formed 2 Si phase and Ni 3 Si 2 The phase reaches the purpose of regulating and controlling microstructure and further improving the performance of Cu-Ni-Si alloy.
Compared with the prior art, the invention has the following beneficial effects:
the invention provides an application of a copper alloy strip process for preparing a copper alloy strip with higher strength and hardness and good electric conduction and heat conduction properties in the production of lead frame alloy strips through a two-stage aging heat treatment process. The method controls the strip forming and the two-stage aging heat treatment system, and the obtained strip contains Ni which is finely dispersed and distributed 2 Si and Ni 3 Si 2 The comprehensive performance of the phase and alloy is effectively improved, and the obtained material has the optimal performance reaching the tensile strength of 722MPa, the elongation of 3.9 percent and the Vickers hardness of 226.9N.mm -2 Conductivity 21.42% IACS and thermal conductivity 190.1 W.m -1 ·K -1
Drawings
FIG. 1 is an optical micrograph of a Cu-Ni-Si alloy of a lead frame in examples 1 to 4 of the present invention.
Fig. 2 is a scanning electron micrograph of a Cu-Ni-Si alloy of the lead frame in examples 1 to 4 of the present invention.
Fig. 3 is a scanning electron micrograph of a Cu-Ni-Si alloy of the lead frame of example 3 of the present invention.
(a) As a whole morphology, it can be seen that two fine second phases having significant differences in contrast to the copper matrix are formed near the grain boundary in example 3, one being a flaky particle phase and one being a spherical particle phase, and the alloy matrix being at the marked point a in (a); the flaky particulate phase described in (a) at label point B; the spherical particulate phase described in (a) at marker point C in (C).
It can be seen from fig. 1 that only a small amount of the second phase precipitated near the grain boundary in examples 1 and 2, and a large amount of fine dispersed second phase particles precipitated in examples 3 and 4 as the temperature of the second aging heat treatment increased.
As can be seen from fig. 2, in examples 1 and 2, flaky grain phases were precipitated, and the precipitated phases were distributed in the vicinity of grain boundaries; in examples 3 and 4, flaky grain phases and spherical grain phases were precipitated, and the precipitated phases were distributed near and in the grain boundaries.
Detailed Description
The invention is further specifically described below in connection with specific embodiments, with the following pointed out: the following examples are only for illustrating the embodiments of the present invention and are not intended to limit the scope of the claims.
Example 1
The Cu-Ni-Si alloy for the lead frame provided by the embodiment comprises the following materials in percentage by mass: 2.4wt.% Ni, 0.6wt.% Si, 0.2wt.% Mg, 0.01wt.% Zn and the balance copper. After removing oxide skin on the surface of the material, firstly adding Cu and Ni into a smelting furnace, heating to 1300 ℃ for melting, adding pure Si and fully stirring after the copper liquid is melted, then preserving heat for 15min, adding pure Mg and pure Zn, and pouring into ingots (200 multiplied by 81 multiplied by 20 mm) after stirring; then heating to 925 ℃, preserving heat for 2 hours, and hot-rolling into a plate strip with the thickness of 4mm, wherein the hot-rolling reduction rate is 80%; immediately water-cooling, softening and annealing at 550 ℃, and preserving heat for 6 hours; performing primary cold rolling with the rolling reduction of 65%, and rolling the plate strip to 1.4mm; solid solution is carried out, the temperature is 970 ℃, and the heat preservation is carried out for 1h; performing secondary cold rolling with the rolling reduction of 50%, and rolling the plate strip to 0.7mm; performing primary aging heat treatment at 150 ℃ for 6 hours; performing secondary aging heat treatment at 400 ℃ for 2 hours; rolling a finished product, and stretch bending and straightening; finally heating to 360 ℃ for heat preservation for 5 hours, cooling to room temperature, and finishing stress relief annealing.
Example 2
The Cu-Ni-Si alloy for the lead frame provided by the embodiment comprises the following materials in percentage by mass: 2.4wt.% Ni, 0.6wt.% Si, 0.2wt.% Mg, 0.01wt.% Zn and the balance copper. After removing oxide skin on the surface of the material, firstly adding Cu and Ni into a smelting furnace, heating to 1300 ℃ for melting, adding pure Si and fully stirring after the copper liquid is melted, then preserving heat for 15min, adding pure Mg and pure Zn, and pouring into ingots (198 multiplied by 83 multiplied by 20 mm) after stirring; then heating to 925 ℃, preserving heat for 2 hours, and hot-rolling into a plate strip with the thickness of 4mm, wherein the hot-rolling reduction rate is 80%; immediately water-cooling, softening and annealing at 550 ℃, and preserving heat for 6 hours; performing primary cold rolling with the rolling reduction of 65%, and rolling the plate strip to 1.4mm; solid solution is carried out, the temperature is 970 ℃, and the heat preservation is carried out for 1h; performing secondary cold rolling with the rolling reduction of 50%, and rolling the plate strip to 0.7mm; performing primary aging heat treatment at 150 ℃ for 6 hours; performing secondary aging heat treatment at 450 ℃ for 2 hours; rolling a finished product, and stretch bending and straightening; finally heating to 360 ℃ for heat preservation for 5 hours, cooling to room temperature, and finishing stress relief annealing.
Example 3
The Cu-Ni-Si alloy for the lead frame provided by the embodiment comprises the following materials in percentage by mass: 2.4wt.% Ni, 0.6wt.% Si, 0.2wt.% Mg, 0.01wt.% Zn and the balance copper. After removing oxide skin on the surface of the material, firstly adding Cu and Ni into a smelting furnace, heating to 1300 ℃ for melting, adding pure Si and fully stirring after the copper liquid is melted, then preserving heat for 15min, adding pure Mg and pure Zn, and pouring into ingots (202 multiplied by 76 multiplied by 20 mm) after stirring; then heating to 925 ℃, preserving heat for 2 hours, and hot-rolling into a plate strip with the thickness of 4mm, wherein the hot-rolling reduction rate is 80%; immediately water-cooling, softening and annealing at 550 ℃, and preserving heat for 6 hours; performing primary cold rolling with the rolling reduction of 65%, and rolling the plate strip to 1.4mm; solid solution is carried out, the temperature is 970 ℃, and the heat preservation is carried out for 1h; performing secondary cold rolling with the rolling reduction of 50%, and rolling the plate strip to 0.7mm; performing primary aging heat treatment at 150 ℃ for 6 hours; performing secondary aging heat treatment at 500 ℃ for 2 hours; rolling a finished product, and stretch bending and straightening; finally heating to 360 ℃ for heat preservation for 5 hours, cooling to room temperature, and finishing stress relief annealing.
It can be seen from fig. 3 (a), that two fine second phases having a significant difference in contrast to the copper matrix are formed near the grain boundary in example 3, one being a flaky particle phase and one being a spherical particle phase, and the alloy matrix being at the mark point a in fig. 3 (a); at point B in fig. 3 (B) is the flaky particulate phase depicted in fig. 3 (a); at marked point C in fig. 3 (C) is the spherical particulate phase described in fig. 3 (a).
Table 1 shows the point sweep spectra of the Cu-Ni-Si alloy of the lead frame in example 3 of the present invention, and the specific component point positions are shown in FIG. 3. By comparing the elemental composition at the mark point A, B, C, it can be determined that the alloy matrix is at the mark point A in FIG. 3 (a), and Ni is at the mark point B in FIG. 3 (B) 2 Si phase, ni at marked point C in FIG. 3 (C) 3 Si 2 And (3) phase (C).
TABLE 1 Point sweep Spectrum of lead frame Cu-Ni-Si alloy in example 3
Example 4
The Cu-Ni-Si alloy for the lead frame provided by the embodiment comprises the following materials in percentage by mass: 2.4wt.% Ni, 0.6wt.% Si, 0.2wt.% Mg, 0.01wt.% Zn and the balance copper. After removing oxide skin on the surface of the material, firstly adding Cu and Ni into a smelting furnace, heating to 1300 ℃ for melting, adding pure Si and fully stirring after the copper liquid is melted, then preserving heat for 15min, adding pure Mg and pure Zn, and pouring into ingots (200 multiplied by 80 multiplied by 20 mm) after stirring; then heating to 925 ℃, preserving heat for 2 hours, and hot-rolling into a plate strip with the thickness of 4mm, wherein the hot-rolling reduction rate is 80%; immediately water-cooling, softening and annealing at 550 ℃, and preserving heat for 6 hours; performing primary cold rolling with the rolling reduction of 65%, and rolling the plate strip to 1.4mm; solid solution is carried out, the temperature is 970 ℃, and the heat preservation is carried out for 1h; performing secondary cold rolling with the rolling reduction of 50%, and rolling the plate strip to 0.7mm; performing primary aging heat treatment at 150 ℃ for 6 hours; performing secondary aging heat treatment at 550 ℃ for 2 hours; rolling a finished product, and stretch bending and straightening; finally heating to 360 ℃ for heat preservation for 5 hours, cooling to room temperature, and finishing stress relief annealing.
The properties of the Cu-Ni-Si lead frames prepared in all examples are shown in Table 2.
Table 2 correlation properties of all examples
The correlation properties of examples 1-4 are compared, and it can be seen that the combination property of example 3 is best, and is characterized in that it has the highest yield strength, tensile strength, elongation and hardness, and the conductivity, elongation and thermal conductivity can basically meet the use requirements.
Although preferred embodiments have been shown and described in detail herein, it will be apparent to those skilled in the art that various changes and modifications can be made therein without departing from the spirit of the invention, which is deemed to be within the scope of the invention as defined in the following claims.

Claims (5)

1. The preparation method of the Cu-Ni-Si alloy for the lead frame is characterized by comprising the following steps of: 2.4% of Ni, 0.6% of Si, 0.2% of Mg, 0.01% of Zn, and the balance of copper and unavoidable impurities. The preparation process of the alloy comprises the following steps:
smelting, hot rolling, softening annealing, primary cold rolling, solid solution, secondary cold rolling, primary aging heat treatment, secondary aging heat treatment, rolling finished products, stretch bending straightening and stress relief annealing, and the method specifically comprises the following steps:
(1) According to the content of 2.4 percent of Ni, 0.6 percent of Si, 0.2 percent of Mg and 0.01 percent of Zn, in the copper alloy composition, cu adopts electrolytic Cu, ni adopts electrolytic Ni, si adopts pure Si, mg adopts pure Mg, zn adopts pure Zn, and oxide skin on the surface is weighed and removed according to the mass percentage;
(2) Smelting: adding the electrolytic Cu and the electrolytic Ni in the step (1) into a smelting furnace, and heating to 1300 DEG C
Melting, adding pure Si after the copper liquid is melted, fully stirring, then preserving heat for 15min, adding pure Mg and pure Zn, and pouring into ingots after stirring;
(3) And (3) hot rolling: heating the cast ingot obtained in the step (2) to 925 ℃, preserving heat for 2 hours, and then rolling, wherein the hot rolling reduction rate is 80%;
(4) Softening and annealing: immediately water-cooling the plate strip obtained in the step (3), then heating to 550 ℃ and preserving heat for 6 hours, wherein the annealing process adopts reducing gas for protection;
(5) Primary cold rolling: cold rolling the sheet material obtained in the step (4), wherein the primary cold rolling reduction is 65%;
(6) Solid solution: carrying out solid solution treatment on the plate obtained in the step (5) by adopting an air cushion annealing furnace, wherein the solid solution temperature is 970 ℃, the heat preservation time is 1h, and reducing gas is adopted for protection in the solid solution process;
(7) Secondary cold rolling: cold rolling the sheet material obtained in the step (6), wherein the secondary cold rolling reduction rate is 50%;
(8) Primary aging heat treatment: heating the plate obtained in the step (7) to 150 ℃ and preserving heat for 6 hours;
(9) And (3) secondary aging heat treatment: heating the plate obtained in the step (8) to 400-550 ℃ and preserving heat for 2h;
(10) And (3) rolling a finished product: cold rolling the sheet material obtained in the step (9), wherein the rolling reduction of the finished product is about 30%;
(11) Stretch bending and straightening: stretch bending and straightening are carried out on the plate obtained in the step (10);
(12) Stress relief annealing: heating the plate in the step (11) to 360 ℃, preserving heat for 5 hours, and naturally cooling to room temperature.
2. The method of claim 1, wherein the purity of the electrolytic Cu, electrolytic Ni, pure Si, pure Mg and pure Zn in step (1) is 99.9% or more.
3. The method according to claim 1, wherein Ni and Si in the alloy are precipitated with finely dispersed Ni 2 And Si phase.
4. The method according to claim 1, wherein the secondary aging temperature in step (9) is 500 to 550 ℃.
5. The method according to claim 4, wherein the Ni and Si element precipitated phases in the alloy are other than Ni having fine dispersion 2 Si phase and Ni 3 Si 2 And (3) phase (C).
CN202310465955.3A 2023-04-26 2023-04-26 Cu-Ni-Si alloy material for lead frame and preparation method thereof Pending CN116640961A (en)

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Application Number Priority Date Filing Date Title
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