CN108823466B - Multi-element composite precipitation strengthening type high-strength high-conductivity copper alloy and preparation method thereof - Google Patents
Multi-element composite precipitation strengthening type high-strength high-conductivity copper alloy and preparation method thereof Download PDFInfo
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Abstract
The invention relates to a multi-element composite precipitation strengthening type high-strength high-conductivity copper alloy and a preparation method thereof, belonging to the technical field of metal material preparation and processing. The alloy comprises the following components in percentage by mass: 1.0 to 6.0% of Ni, 0.2 to 1.5% of Si, 0.1 to 0.5% of Zn, 0.1 to 0.5% of Cr, 0.01 to 0.1% of P, the total content of inevitable impurity elements is less than 0.1%, and the balance of Cu. The preparation process comprises the following steps: fusion casting → homogenization → hot rolling → double-sided milling → rough cold rolling → trimming → primary on-line quenching → pre-finish rolling → secondary on-line quenching → primary finish rolling → primary aging → secondary finish rolling → secondary aging. After secondary aging, the alloy has the strength of more than 800MPa, the conductivity of more than 50 percent IACS, and a precipitated phase of-Ni2Si and a complex precipitate phase containing Cu, Ni, Si, Cr and P elements. The invention has the advantages of easy smelting, composite precipitation strengthening, high tensile strength, high conductivity and the like.
Description
Technical Field
The invention relates to a novel multi-element high-strength high-conductivity copper alloy and a preparation method thereof, belongs to the technical field of metal material preparation and processing, and particularly provides a composition and a preparation method of a composite precipitation-strengthened high-strength high-conductivity Cu-Ni-Si-Zn-Cr-P alloy.
Background
With the rapid development of information technology, integrated circuits are developed to a very large or huge scale, and the requirements of higher strength and higher conductivity are put forward on the performance of lead frame copper alloy. So far, the lead frame copper alloys which have been widely put into practical use mainly include Cu-Fe-P system alloys, Cu-Ni-Si system alloys, and Cu-Cr-Zr system alloys. The Cu-Fe-P series alloy is a medium-strength high-conductivity type copper alloy which is most widely applied, but has the problems of poor brazing heat-resistant stripping resistance, low strength, magnetic property of the alloy and the like; the Cu-Cr-Zr alloy is considered to be the most promising high-strength and high-conductivity copper alloy, the conductivity of the Cu-Cr-Zr alloy can reach 80% IACS, the tensile strength is more than 600MPa, but the Cu-Cr-Zr alloy needs vacuum melting and is difficult to prepare and process, and the large-scale application of the Cu-Cr-Zr alloy is limited. The Cu-Ni-Si alloy has no magnetism, is easy to melt, has good brazing performance, higher strength and good conductivity, and is the mainstream development direction of the high-strength and high-conductivity copper alloy for the lead frame in the world at present.
The main approach for developing high-strength and high-conductivity copper alloy is microalloying, i.e. adding a certain amount of alloy elements with low solid solubility into a copper matrix, and precipitating a large amount of second phases from the copper matrix through solution treatment and aging treatment, so as to improve the strength of the alloy without greatly reducing the conductivity. For example: the C70250 copper alloy is a strong aging precipitation strengthening type copper alloy formed by adding trace Zn and Mg on the basis of Cu-Ni-Si alloy, the tensile strength of the copper alloy can reach 750MPa, and the electric conductivity of the copper alloy is about 40 percent IACS; c70350 is prepared by adding a trace amount of Co to C70250, and the tensile strength of the alloy can reach 800MPa, but the conductivity of the alloy is greatly reduced and is about 35% IACS. The alloy is difficult to meet the performance requirements (tensile strength is more than 800MPa, and conductivity is more than 50% IACS) of the copper alloy for the lead frame of the next generation of the extremely large or large scale integrated circuit.
Disclosure of Invention
Aiming at the current situation that the strength and the electric conductivity of the existing high-strength high-conductivity copper alloy are difficult to simultaneously meet the performance requirements of the next generation of lead frame materials of the very large or large scale integrated circuit, the invention develops the multielement composite precipitation strengthening type high-strength high-conductivity copper alloy with the tensile strength of more than 800MPa and the electric conductivity of more than 50 percent IACS and the preparation process thereof so as to meet the performance requirements of the next generation of lead frame materials of the very large or large scale integrated circuit.
A multi-element composite precipitation strengthening type high-strength high-conductivity copper alloy is characterized in that the alloy comprises the following components in percentage by mass: 1.0 to 6.0 percent of Ni, 0.2 to 1.5 percent of Si, 0.1 to 0.5 percent of Zn, 0.1 to 0.5 percent of Cr, 0.01 to 0.1 percent of P, the total content of inevitable impurity elements is not higher than 0.1 percent, and the balance of Cu.
Furthermore, other elements with the content of 0.01-0.5% can be added according to the needs, and the other elements are Mg, Zr, Ti, B, Al, Co, Fe, Sn and rare earth elements.
The preparation method of the multi-element composite precipitation strengthening high-strength high-conductivity copper alloy comprises the following specific preparation steps:
(1) casting: proportionally mixing electrolytic Cu with the purity of more than 99.96%, electrolytic Ni with the purity of more than 99.96% and polycrystalline Si with the purity of more than 99.99% in a smelting furnace, heating to 1250-1350 ℃, and covering charcoal on the surface of metal to prevent oxidation according to needs; after the Cu-Ni-Si is completely melted, adding pure Cr blocks with the purity of more than 99.99 percent, CuP14 intermediate alloy and 65 brass into the molten metal; standing the smelted alloy melt for 10-30 minutes, and removing slag, wherein the temperature is kept at 1200-1350 +/-10 ℃; then casting into a flat ingot, and removing surface defects after cooling to room temperature;
(2) carrying out homogenization treatment;
(3) hot rolling;
(4) milling on two sides: performing double-sided milling according to the requirement to remove the defects on the surface of the hot-rolled plate, wherein the milling depth is 0.1-0.5 mm;
(5) rough cold rolling;
(6) trimming: cutting off 2-10 mm of the edge of the plate after rough cold rolling according to the edge crack condition;
(7) primary on-line quenching;
(8) pre-finish rolling;
(9) secondary on-line quenching;
(10) primary finish rolling;
(11) primary aging;
(12) secondary finish rolling;
(13) secondary aging;
further, the homogenization treatment is characterized in that: and (3) preserving the heat of the slab ingot for 1-8 hours at 850-1000 ℃ in a protective atmosphere.
Further, 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 rolling reduction of hot rolling passes is 20-50%, and the total deformation is 50-90%.
Further, the rough cold rolling is characterized in that: the pass deformation is 15-40%, the total deformation is 40-90%, and the thickness after rolling is 1.0-2.0 mm.
Further, the primary online quenching is characterized in that: the temperature is 900-1000 ℃, and the speed is 1-10 m/min; the secondary on-line quenching is characterized in that: the temperature is 900-1000 ℃, and the speed is 2-20 m/min.
Further, the pre-finish rolling is characterized in that: the pass deformation is 15-50%, the total deformation is 50-90%, and the thickness after rolling is 0.5-1.5 mm.
Further, the primary finish rolling is characterized in that: the pass deformation is 15-35%, the total deformation is 30-80%, and the thickness after rolling is 0.1-0.5 mm; the secondary finish rolling is characterized in that: the pass deformation is 15-30%, the total deformation is 20-70%, and the thickness after rolling is 0.05-0.3 mm.
Further, the primary aging and the secondary aging are characterized in that: and (3) ageing the bell-type furnace, keeping the temperature at 350-550 ℃ for 1-5 hours in a protective atmosphere.
Furthermore, after the composite precipitation strengthening type high-strength high-conductivity copper alloy is subjected to aging precipitation, precipitated phases mainly comprise-Ni 2Si with the diameter of 10-30 nm and complex precipitated phases with the diameter of 60-100 nm and containing Cu, Ni, Si, Cr and P elements; the alloy has the characteristics of final performance: tensile strength of not less than 800MPa and electric conductivity of not less than 50% IACS.
The invention has the following advantages: the alloy is easy to melt in the atmosphere, the process is simple and reliable, the composite precipitation strengthening is realized, the tensile strength is high, the conductivity is high, and the like.
Drawings
FIG. 1 shows the morphology of a precipitated phase of a Cu-Ni-Si-Zn-Cr-P alloy.
FIG. 2 is a complex precipitated phase composition spectrum of Cu-Ni-Si-Zn-Cr-P alloy.
FIG. 3 is a Cu-Ni-Si-Zn-Cr-P alloy-Ni 2Si precipitated phase composition spectrum.
FIG. 4 is a process flow for preparing Cu-Ni-Si-Zn-Cr-P alloy.
Detailed Description
Example 1: the invention designs and develops a multi-element composite precipitation strengthening type high-strength high-conductivity copper alloy which meets the performance requirements of a lead frame of a very large or huge integrated circuit: cu-3Ni-0.6Si-0.16Zn-0.15Cr-0.03P, wherein the composite strengthening precipitated phase of the alloy mainly comprises-Ni 2Si with the diameter of about 20nm and a complex precipitated phase which is about 80nm and contains Cu, Ni, Si, Cr and P elements;
the preparation method of the Cu-Ni-Si-Zn-Cr-P alloy is specifically described as follows:
(1) casting: putting the electrolytic Cu (the purity is more than 99.96 percent), the electrolytic Ni (the purity is more than 99.96 percent) and the polycrystalline Si (the purity is more than 99.99 percent) which are prepared in proportion into a smelting furnace, heating to 1250-1350 ℃, and covering a layer of charcoal on the surface of the metal to prevent oxidation; after the alloy is completely melted, preserving the heat for 10 minutes, and then adding pure Cr blocks (the purity is more than 99.99 percent), CuP14 intermediate alloy and 65 brass into the molten metal; finally, the alloy gold comprises the following components in percentage by mass: 3% of Ni, 0.6% of Si, 0.16% of Zn, 0.15% of Cr, 0.03% of P, less than 0.1% of the total content of inevitable impurity elements and the balance of Cu. Standing the smelted alloy melt for 10 minutes, and then removing slag, wherein the temperature is kept at 1250 +/-10 ℃; and then casting into a flat ingot, and removing surface defects after cooling to room temperature.
(2) Homogenizing: and preserving the temperature of the slab ingot with the surface defects removed for 3 hours at 950 ℃ in a protective atmosphere.
(3) Hot rolling: and (3) carrying out hot rolling deformation on the homogenized blank, wherein the initial rolling temperature is 900 ℃, the final rolling temperature is 780 ℃, the reduction of hot rolling pass is 50%, and the total deformation is 80%.
(4) Milling on two sides: and removing the defects on the surface of the hot-rolled plate, and milling to a depth of 0.3 mm.
(5) Rough cold rolling: pass deformation is 30%, total deformation is 60%, and the thickness after rolling is 1.2 mm.
(6) Trimming: in order to eliminate the adverse effect of the rolling edge crack, the two side edge parts of the plate after rough cold rolling are cut off by 5 mm.
(7) Primary on-line quenching: the temperature was 950 ℃ and the speed was 8 m/min.
(8) Pre-finish rolling: the pass deformation is 20 percent, the total deformation is 66.7 percent, and the thickness is 0.8 mm.
(9) Secondary on-line quenching: the temperature was 930 ℃ and the speed was 15 m/min.
(10) Primary finish rolling: the pass deformation is 20 percent, the total deformation is 50 percent, and the thickness after rolling is 0.4 mm.
(11) Primary aging: the bell-type furnace is aged, protected at 475 ℃ and kept warm for 4 hours.
(12) Secondary finish rolling: pass deformation is 20%, total deformation is 50%, and the thickness after rolling is 0.2 mm.
(13) Secondary aging: the bell-type furnace is aged, the protective atmosphere is kept at the temperature of 450 ℃, and the heat is preserved for 4 hours. The alloy after aging has the tensile strength of 804.8MPa and the conductivity of 51.2 percent IACS.
Example 2: the invention designs and develops a multi-element composite precipitation strengthening type high-strength high-conductivity copper alloy which meets the performance requirements of a lead frame of a very large or huge integrated circuit: cu-3.05Ni-0.88Si-0.57Zn-0.31Cr-0.04P, wherein the composite strengthening precipitated phase of the alloy mainly comprises-Ni 2Si with the diameter of about 20nm and a complex precipitated phase which is about 80nm and contains Cu, Ni, Si, Cr and P elements;
the preparation method of the Cu-Ni-Si-Zn-Cr-P alloy is specifically described as follows:
(1) casting: putting the electrolytic Cu (the purity is more than 99.96 percent), the electrolytic Ni (the purity is more than 99.96 percent) and the polycrystalline Si (the purity is more than 99.99 percent) which are prepared in proportion into a smelting furnace, heating to 1250-1350 ℃, and covering a layer of charcoal on the surface of the metal to prevent oxidation; after the alloy is completely melted, preserving the heat for 10 minutes, and then adding pure Cr blocks (the purity is more than 99.99 percent), CuP14 intermediate alloy and 65 brass into the molten metal; finally, the alloy gold comprises the following components in percentage by mass: 3% of Ni, 0.6% of Si, 0.16% of Zn, 0.15% of Cr, 0.03% of P, less than 0.1% of the total content of inevitable impurity elements and the balance of Cu. Standing the smelted alloy melt for 10 minutes, and then removing slag, wherein the temperature is kept at 1250 +/-10 ℃; and then casting into a flat ingot, and removing surface defects after cooling to room temperature.
(2) Homogenizing: and preserving the temperature of the slab ingot with the surface defects removed for 3 hours at 950 ℃ in a protective atmosphere.
(3) Hot rolling: and (3) carrying out hot rolling deformation on the homogenized blank, wherein the initial rolling temperature is 900 ℃, the final rolling temperature is 780 ℃, the reduction of hot rolling pass is 50%, and the total deformation is 80%.
(4) Milling on two sides: and removing the defects on the surface of the hot-rolled plate, and milling to a depth of 0.3 mm.
(5) Rough cold rolling: pass deformation is 30%, total deformation is 60%, and the thickness after rolling is 1.2 mm.
(6) Trimming: in order to eliminate the adverse effect of the rolling edge crack, the two side edge parts of the plate after rough cold rolling are cut off by 5 mm.
(7) Primary on-line quenching: the temperature was 950 ℃ and the speed was 8 m/min.
(8) Pre-finish rolling: the pass deformation is 20 percent, the total deformation is 66.7 percent, and the thickness is 0.8 mm.
(9) Secondary on-line quenching: the temperature was 930 ℃ and the speed was 15 m/min.
(10) Primary finish rolling: the pass deformation is 20 percent, the total deformation is 50 percent, and the thickness after rolling is 0.4 mm.
(11) Primary aging: the bell-type furnace is aged, protected at 475 ℃ and kept warm for 4 hours.
(12) Secondary finish rolling: pass deformation is 20%, total deformation is 50%, and the thickness after rolling is 0.2 mm.
(13) Secondary aging: the bell-type furnace is aged, the protective atmosphere is kept at the temperature of 450 ℃, and the heat is preserved for 4 hours. The alloy after aging has the tensile strength of 800.8MPa and the conductivity of 50.2 percent IACS.
Example 3: the invention designs and develops a multi-element composite precipitation strengthening type high-strength high-conductivity copper alloy which meets the performance requirements of a lead frame of a very large or huge integrated circuit: cu-3.28Ni-0.60Si-0.22Zn-0.11Cr-0.036P, wherein the composite strengthening precipitated phase of the alloy mainly comprises-Ni 2Si with the diameter of about 20nm and a complex precipitated phase which is about 80nm and contains Cu, Ni, Si, Cr and P elements;
the preparation method of the Cu-Ni-Si-Zn-Cr-P alloy is specifically described as follows:
(1) casting: putting the electrolytic Cu (the purity is more than 99.96 percent), the electrolytic Ni (the purity is more than 99.96 percent) and the polycrystalline Si (the purity is more than 99.99 percent) which are prepared in proportion into a smelting furnace, heating to 1250-1350 ℃, and covering a layer of charcoal on the surface of the metal to prevent oxidation; after the alloy is completely melted, preserving the heat for 10 minutes, and then adding pure Cr blocks (the purity is more than 99.99 percent), CuP14 intermediate alloy and 65 brass into the molten metal; finally, the alloy gold comprises the following components in percentage by mass: 3% of Ni, 0.6% of Si, 0.16% of Zn, 0.15% of Cr, 0.03% of P, less than 0.1% of the total content of inevitable impurity elements and the balance of Cu. Standing the smelted alloy melt for 10 minutes, and then removing slag, wherein the temperature is kept at 1250 +/-10 ℃; and then casting into a flat ingot, and removing surface defects after cooling to room temperature.
(2) Homogenizing: and preserving the temperature of the slab ingot with the surface defects removed for 3 hours at 950 ℃ in a protective atmosphere.
(3) Hot rolling: and (3) carrying out hot rolling deformation on the homogenized blank, wherein the initial rolling temperature is 900 ℃, the final rolling temperature is 780 ℃, the reduction of hot rolling pass is 50%, and the total deformation is 80%.
(4) Milling on two sides: and removing the defects on the surface of the hot-rolled plate, and milling to a depth of 0.3 mm.
(5) Rough cold rolling: pass deformation is 30%, total deformation is 60%, and the thickness after rolling is 1.2 mm.
(6) Trimming: in order to eliminate the adverse effect of the rolling edge crack, the two side edge parts of the plate after rough cold rolling are cut off by 5 mm.
(7) Primary on-line quenching: the temperature was 950 ℃ and the speed was 8 m/min.
(8) Pre-finish rolling: the pass deformation is 20 percent, the total deformation is 66.7 percent, and the thickness is 0.8 mm.
(9) Secondary on-line quenching: the temperature was 930 ℃ and the speed was 15 m/min.
(10) Primary finish rolling: the pass deformation is 20 percent, the total deformation is 50 percent, and the thickness after rolling is 0.4 mm.
(11) Primary aging: the bell-type furnace is aged, protected at 475 ℃ and kept warm for 4 hours.
(12) Secondary finish rolling: pass deformation is 20%, total deformation is 50%, and the thickness after rolling is 0.2 mm.
(13) Secondary aging: the bell-type furnace is aged, the protective atmosphere is kept at the temperature of 450 ℃, and the heat is preserved for 4 hours. The alloy after aging has the tensile strength of 825.6MPa and the conductivity of 50.7 percent IACS.
Claims (10)
1. A multi-element composite precipitation strengthening type high-strength high-conductivity copper alloy is characterized in that the alloy comprises the following components in percentage by mass: 3.0 to 6.0 percent of Ni, 0.2 to 1.5 percent of Si, 0.1 to 0.5 percent of Zn, 0.1 to 0.5 percent of Cr, 0.01 to 0.1 percent of P, the total content of inevitable impurity elements is not higher than 0.1 percent, and the balance of Cu;
the main preparation and processing technology of the alloy comprises the following steps: casting, homogenizing treatment, 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 and secondary aging; the multielement composite precipitation strengthening type high-strength high-conductivity copper alloy with the tensile strength of more than 800MPa and the electric conductivity of more than 50 percent IACS is obtained after the preparation and processing of the process; and form de-Ni in the alloy2Besides the Si precipitated phase, a complex precipitated phase containing Ni, Si, Cr, Zn and P is formed; the precipitated phase mainly comprises-Ni 2Si with the diameter of 10-30 nm and a complex precipitated phase with the diameter of 60-100 nm and containing Cu, Ni, Si, Cr and P elements.
2. The multi-element composite precipitation strengthening type high-strength high-conductivity copper alloy as claimed in claim 1, wherein the other elements are added in an amount of 0.01-0.5%, and the other elements are Mg, Zr, Ti, B, Al, Co, Fe, Sn and rare earth elements.
3. A method for producing the copper alloy according to claim 1 or 2, characterized by comprising the steps of:
(1) casting: proportionally mixing electrolytic Cu with the purity of more than 99.96%, electrolytic Ni with the purity of more than 99.96% and polycrystalline Si with the purity of more than 99.99% in a smelting furnace, heating to 1250-1350 ℃, and covering charcoal on the surface of metal to prevent oxidation according to needs; after the Cu-Ni-Si is completely melted, adding pure Cr blocks with the purity of more than 99.99 percent, CuP14 intermediate alloy and 65 brass into the molten metal; standing the smelted alloy melt for 10-30 minutes, and removing slag, wherein the temperature is kept at 1200-1350 ℃; then casting into a flat ingot, and removing surface defects after cooling to room temperature;
(2) carrying out homogenization treatment; keeping the temperature of the slab ingot at 850-1000 ℃ for 1-8 hours in a protective atmosphere;
(3) hot rolling;
(4) milling on two sides: performing double-sided milling according to the requirement to remove the defects on the surface of the hot-rolled plate, wherein the milling depth is 0.1-0.5 mm;
(5) rough cold rolling;
(6) trimming: cutting off 2-10 mm of the edge of the plate after rough cold rolling according to the edge crack condition;
(7) primary on-line quenching;
(8) pre-finish rolling;
(9) secondary on-line quenching;
(10) primary finish rolling;
(11) primary aging;
(12) secondary finish rolling;
(13) and (5) secondary aging.
4. The method for producing a copper alloy according to claim 3, wherein said hot rolling is characterized by: the initial rolling temperature is more than or equal to 850 ℃, the final rolling temperature is more than or equal to 700 ℃, the rolling reduction of hot rolling passes is 20-50%, and the total deformation is 50-90%.
5. The method for preparing a copper alloy according to claim 3, wherein said rough cold rolling is characterized by: the pass deformation is 15-40%, the total deformation is 40-90%, and the thickness after rolling is 1.0-2.0 mm.
6. The method for producing a copper alloy according to claim 3, wherein the primary on-line quenching is characterized by: the temperature is 900-1000 ℃, and the speed is 1-10 m/min; the secondary on-line quenching is characterized in that: the temperature is 900-1000 ℃, and the speed is 2-20 m/min.
7. The method for producing a copper alloy according to claim 3, wherein said pre-finish rolling is characterized by: the pass deformation is 15-50%, the total deformation is 50-90%, and the thickness after rolling is 0.5-1.5 mm.
8. The method of manufacturing a copper alloy according to claim 3, wherein said primary finish rolling is characterized by: the pass deformation is 15-35%, the total deformation is 30-80%, and the thickness after rolling is 0.1-0.5 mm; the secondary finish rolling is characterized in that: the pass deformation is 15-30%, the total deformation is 20-70%, and the thickness after rolling is 0.05-0.3 mm.
9. A method of producing a copper alloy according to claim 3, wherein said primary aging and secondary aging are characterized by: and (3) ageing the bell-type furnace, keeping the temperature at 350-550 ℃ for 1-5 hours in a protective atmosphere.
10. The preparation method of the copper alloy according to claim 3, wherein after aging precipitation, the precipitation phases mainly comprise-Ni 2Si with the diameter of 10-30 nm and complex precipitation phases with the diameter of 60-100 nm and containing Cu, Ni, Si, Cr and P elements; the alloy has the characteristics of final performance: tensile strength of not less than 800MPa and electric conductivity of not less than 50% IACS.
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| US7090732B2 (en) * | 2000-12-15 | 2006-08-15 | The Furukawa Electric, Co., Ltd. | High-mechanical strength copper alloy |
| JP4785092B2 (en) * | 2007-11-05 | 2011-10-05 | 古河電気工業株式会社 | Copper alloy sheet |
| CN107794406B (en) * | 2017-10-16 | 2019-05-17 | 北京科技大学 | A kind of production technology of high-strength highly-conductive corson alloy |
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