CN1563447A - Dispersion strengthened copper alloy, and preparing technical method - Google Patents

Dispersion strengthened copper alloy, and preparing technical method Download PDF

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Publication number
CN1563447A
CN1563447A CN 200410029836 CN200410029836A CN1563447A CN 1563447 A CN1563447 A CN 1563447A CN 200410029836 CN200410029836 CN 200410029836 CN 200410029836 A CN200410029836 A CN 200410029836A CN 1563447 A CN1563447 A CN 1563447A
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copper
alloy
preparation technology
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powder
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CN1291049C (en
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宋厚启
牛立业
何伯恂
曹先杰
孟惠娟
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Zhonglu Luoyang Copper Industry Co., Ltd.
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LUOYANG COPPER PROCESSING GROUP CO Ltd
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Abstract

A dispersion intensified copper alloy characterizes that the distribution ratio of the Al content is 0.05-0.6%, the rest is copper and the impurities are more than 0.5%, nitrogen or high pressure atomized water are utilized to prepare Cu-Al alloy powders by oxygen source preparation-materials mixing-cold isostatic pressure-comprehensive heat process-extrusion-cold process-performance test.

Description

Dispersion strengthening copper alloy and preparation technology's method thereof
Technical field:
The present invention relates to microwave tube, resistance welding electrode, circuit lead frame material technology field, a kind of dispersion strengthening copper alloy and preparation technology's method thereof.
Technical background:
Along with the develop rapidly of microwave electron technology, microwave tube seems important day by day to the vital role of modernization of weaponry, and development novel microwave electron tube is needs of realizing the modernization of national defense, develop high-tech.Be used for 052 warship Primary Component microwave tube, the past is used oxygenless copper material, because its physical strength is low, especially behind the high temperature annealing in hydrogen atmosphere, intensity is poorer, can't be used to processing as magnetron inner chamber body, some vital parts of tuning ring.
Usually be used as the common oxygen free copper of microwave tube structured material, though good conduction, heat conductivility and good processing properties are arranged, but because its high temperature resistance softening performance is poor, the electronic element of not competent microwave tube and so on is to the requirement of structured material, microwave tube operating frequency height requires very strict to its accessory size.In the tubulation process, to stand soldering, the pyroprocessing of degasification in addition above 900 ℃, some microwave tube, camera carries the small microwave electron tube on radar, guided missile and the man-made satellite, also will bear the effect of impact, high-frequency vibration and the centrifugal acceleration of acceleration when operation.Therefore, need a kind of high conduction, thermal conductivity that had both kept copper always, have the novel alloy of higher anti-softening temperature again.Usually habitual its softening temperature of solid solution strengthened alloy generally is no more than 600 ℃, and its electric conductivity also is no more than 85%IACS.
At present, inner oxidation method and mechanical alloying method are mainly adopted in commercially producing of high-strength both at home and abroad, high conduction strengthened dispersion copper alloy.Traditional inner oxidation method production dispersion strengthening copper alloy technical process is long, cost is high, labour intensity is big, and difficult quality control.
Summary of the invention:
The purpose of this invention is to provide a kind of dispersion strengthening copper alloy and preparation technology's method thereof, make it simplify the technical matters flow process, reduce production costs, cost descends more than 1/3rd, reduces labour intensity, improves the over-all properties of the finished product.
The objective of the invention is to realize with following technical scheme:
Described dispersion strengthening copper alloy, the content of its aluminium are 0.05~0.6%, surplus is the partition ratio of copper, foreign matter content ≯ 0.5%; Adopt nitrogen or the hydraulic atomized copper-Al alloy powder-oxygen source making-batch mixing-isostatic cool pressing-comprehensive thermal treatment-extruding-cold working-performance detecting process of producing to be made.
Preparation technology's method of described dispersion strengthening copper alloy adopts nitrogen or the hydraulic atomized copper-Al alloy powder-oxygen source making-batch mixing-isostatic cool pressing-comprehensive thermal treatment-extruding-cold working-performance detecting process of producing to make softening, high-strength, the high conduction strengthened dispersion copper alloy of high temperature resistance; With high purity anaerobic electrolytic copper, copper-30% aluminium intermediate alloy, copper-13% phosphorus master alloy reductor is raw material; At first in intermediate frequency furnace, add high-purity anaerobic electrolytic copper melting 10~30 minutes; And then add a little copper-13% phosphorus master alloy deoxidation 0.5~3 minute; Add copper-30% aluminium intermediate alloy melting 3~8 minutes again; Use 0.6~0.8N/mm then 2Nitrogen or 7~9N/mm 2High pressure water carries out powder by atomization.
Preparation technology's method of described dispersion strengthening copper alloy adopted nitrogen or hydraulic atomized copper-Al alloy powder-40~-100 orders of producing, 250-450 ℃ of baking 40~60 hours; Under 600~900 ℃ of nitrogen protections, heated 1~3 hour then, make required oxygen source; The copper-Al alloy powder of oxygen source and atomizing in 1: the ratio of 5-15 was mixed in the V-arrangement mixer 0.5~6 hour, made powder mix; The powder mix that mixes is packed into etc. in the static pressure gum cover, in the isostatic cool pressing oil cylinder, be forced into 100~300N/mm then 2Moulding; To wait the isostatic cool pressing ingot handles 2~6 hours under 700~950 ℃, nitrogen protection after; Reductase 12~8 hour in 750~950 ℃ of hydrogen atmospheres; Sintering 1~5 hour in 900~1000 ℃ of hydrogen atmospheres again.
Preparation technology's method of described dispersion strengthening copper alloy, the powder ingot that comprehensive thermal treatment is finished is extruded into the bar or the tubing of required specification under 750~950 ℃ of temperature.
Preparation technology's method of described dispersion strengthening copper alloy is carried out the product of extruding again 30~90% drawing and is processed into product.
Owing to adopted art scheme as mentioned above, the present invention has following superiority:
Dispersion strengthening copper alloy has very good high temperature resistance softening properties, has favorable conductive, heat conductivility simultaneously concurrently, is strong, the high-conductivity copper alloy of at present a kind of splendid heat; The microwave tube inner chamber body that can successfully be used for systems such as carrier-borne, airborne satellite radar, electronic countermeasure, remote-control romote-sensing, particle accelerator; And the slow wave line of transmitting tube grid steady arm, travelling-wave tubes etc.; And at resistance welding electrode, current-carrying spring, electric contacting piece, as: lead frames such as motor rotor rod, coupling end and supporting pieces, generator lead-in wire, fields such as cast steel crystallizer also are widely adopted.
The present invention adopts AL at existing disperse copper 2O 3Do on the basis of the second particle producing and manufacturing technique, taked the technological measure of some,, set requirement thereby every technical indicator performance is reached as waiting static pressure, high temperature to burn method and swaging and processing parameter:
1), the material resistance to air loss is good, technical process is reasonable, can well improve the strength of materials and cold-forming property, the annealing in hydrogen atmosphere of avoiding material is expanded also the big benefit of committee; Bar tensile strength>430N/mm 2Electric conductivity>90%IACS; Vary in diameter<0.01mm.
Dispersion strengthening copper alloy materials performance after operation is processed as mentioned above is: after the annealing in 30 minutes of 900 ℃ of hydrogen atmospheres, and the tensile strength Rm365N/mm of alloy material 2Yield strength Rp0.2 295N/mm 2Unit elongation A 20%; Radial dimension expansion 0.02mm; And production cost descends 33%.Reach customer requirements fully.
The drawing explanation:
Fig. 1 is a dispersion strengthening copper alloy preparation technology schema:
Embodiment one:
Being used for electrovacuum microwave tube TuMAI0.12 alloy with production is example.Raw material is selected high purity anaerobic electrolytic copper, copper-30% aluminium intermediate alloy, copper-13% phosphorus reductor master alloy for use;
1), nitrogen atomization is produced copper-Al alloy powder: add the high purity electrolytic copper in 100Kw intermediate frequency (IF) smelting stove, wait to melt back melting 15 minutes, add 15 gram copper-13% phosphorus master alloy meltings 1 minute, add copper-30% aluminium intermediate alloy melting 5 minutes again, use 0.75N/mm then 2Nitrogen atomizes, and makes-40 purpose copper-Al alloy powders;
2), oxygen source is made: get-100 order copper-Al alloy powders and be heated to 380 ℃ in resistance furnace, and be incubated 50 hours, required oxygen source was made in heating in 1.5 hours under 840 ℃ of nitrogen protections then;
3), batch mixing: the oxygen source of making mixed in the V-type mixer in 1: 11 ratio with copper-Al alloy powder made powder mix in 3/4 hour;
4), isostatic cool pressing: the powder mix that mixes is packed into etc. in the static pressure gum cover, in the isostatic cool pressing Oil cylinder, be pressurized to 200N/mm then 2Moulding φ 195 * 400mm;
5), comprehensive thermal treatment: etc. the static pressure ingot under 880 ℃ of nitrogen protections, handle and in 900 ℃ of hydrogen atmospheres, reduced 5 hours after 3 hours, sintering 2 hours in 980 ℃ of hydrogen atmospheres again;
6), extruding: the powdered alloy ingot after the comprehensive thermal treatment at 850 ℃ of following extrusion molding φ 40mm alloy bar bases;
7), cold working: the excellent base of φ 40mm is cold drawn to φ 20mm, and the centre need not annealing.
Through the dispersion strengthening copper alloy materials performance after the above operation processing be: after the annealing in 30 minutes of 900 ℃ of hydrogen atmospheres, the tensile strength Rm365N/mm of alloy material 2Yield strength Rp0.2 295N/mm 2Unit elongation A 20%; Radial dimension expansion 0.02mm; And production cost descends 33%.Reach customer requirements fully.
Embodiment two:
Is example to produce 110,000 high voltage isolator conducting rods with the LCM115 alloy, and raw material adopts high purity anaerobic electrolytic copper, copper-30% aluminium intermediate alloy, copper-13% phosphorus reductor master alloy;
1), copper-aluminium dispersion strengthening copper alloy powder is produced in water atomization: add high purity anaerobic electrolytic copper in 100Kw intermediate frequency (IF) smelting stove, wait to melt back melting 15 minutes, add 15 gram copper-13% phosphorus master alloy meltings 1 minute again, add copper-30% aluminium intermediate alloy melting 5 minutes again, use 8.5N/mm then 2High pressure water-100 order copper-Al alloy powders that atomize and make;
2), oxygen source is made: get-100 order copper-Al alloy powders resistance furnace internal heating to 380 ℃ insulation 25 hours, required oxygen source was made in heating in 1.5 hours under 840 ℃ of nitrogen protections then;
3), batch mixing: the oxygen source of making and copper-Al alloy powder mixed in the V-type mixer in 1: 9 ratio made powder mix in 3/4 hour;
4), isostatic cool pressing: the powder mix that mixes packed into etc. is extruded into 200N/mm in the static pressure gum cover in the isostatic cool pressing Oil cylinder 2Moulding φ 195 * 400mm;
5), comprehensive thermal treatment: etc. after the static pressure ingot handled 3 hours under 890 ℃ of nitrogen protections, in 910 ℃ of hydrogen atmospheres, reduced 5 hours, again sintering 2 hours in 980 ℃ of hydrogen atmospheres;
6), extruding: the alloy powder ingot that comprehensive thermal treatment is finished is at the dispersion strengthening copper alloy bar of 850 ℃ of following extrusion molding φ 40mm;
7), cold working: the bar of φ 40mm carried out 75% deformation process to φ 20mm.
Dispersion strengthening copper alloy materials performance after above operation processing is after testing: tensile strength Rm 585N/mm 2, yield strength Rp0.2 564N/mm 2, unit elongation A10.5%, cost descend 34.5%.Reach customer requirements fully.Tensile strength Rm raising about 10%, yield strength Rp0.2 raising about 10%, unit elongation A improve more than 10%.

Claims (7)

1, a kind of dispersion strengthening copper alloy is characterized in that: described dispersion strengthening copper alloy, the content of its aluminium are 0.05~0.6%, surplus is the partition ratio of copper, foreign matter content ≯ 0.5%; Adopt nitrogen or the hydraulic atomized copper-Al alloy powder-oxygen source making-batch mixing-isostatic cool pressing-comprehensive thermal treatment-extruding-cold working-performance detecting process of producing to make softening, high-strength, the high conduction strengthened dispersion copper alloy of high temperature resistance.
2, implement to make preparation technology's method of dispersion strengthening copper alloy as claimed in claim 1, it is characterized in that: described preparation technology's method is a raw material with high purity anaerobic electrolytic copper, copper-30% aluminium intermediate alloy, copper-13% phosphorus master alloy reductor; At first in intermediate frequency furnace, add high-purity anaerobic electrolytic copper melting 10~30 minutes; And then add a little copper-13% phosphorus master alloy deoxidation 0.5~3 minute; Add copper-30% aluminium intermediate alloy melting 3~8 minutes again; Use 0.6~0.8N/mm2 nitrogen or 7~9N/mm then 2High pressure water carries out powder by atomization.
3, preparation technology's method of dispersion strengthening copper alloy as claimed in claim 2 is characterized in that: described preparation technology's method, and atomizing was produced between copper-Al alloy powder-40~-100 orders, 250~450 ℃ of bakings 40~60 hours; Under 600~900 ℃ of nitrogen protections, heated 1~3 hour then, make required oxygen source.
4, preparation technology's method of dispersion strengthening copper alloy as claimed in claim 2, it is characterized in that: described preparation technology's method, the copper-Al alloy powder of oxygen source and atomizing in 1: the ratio of 5-15 was mixed in the V-arrangement mixer 0.5~6 hour, made powder mix; The powder mix that mixes is packed into etc. in the static pressure gum cover, in the isostatic cool pressing oil cylinder, be forced into 100~300N/mm then 2Moulding; After will waiting the isostatic cool pressing ingot under 700~950 ℃, nitrogen protection, to handle 2~6 hours; Reductase 12~8 hour in 750~950 ℃ of hydrogen atmospheres; Sintering 1~5 hour in 900~1000 ℃ of hydrogen atmospheres again.
5, preparation technology's method of dispersion strengthening copper alloy as claimed in claim 2 is characterized in that: described preparation technology's method, and the powder ingot that comprehensive thermal treatment is finished is extruded into the bar or the tubing of required specification under 750~950 ℃ of temperature; The product of extruding are carried out again 30~90% drawing processed finished products.
6, preparation technology's method of dispersion strengthening copper alloy as claimed in claim 2, it is characterized in that: described preparation technology's method, being used for electrovacuum microwave tube TuMAI0.12 alloy with production is example: raw material is selected high purity anaerobic electrolytic copper, copper-30% aluminium intermediate alloy, copper-13% phosphorus reductor master alloy for use;
1), nitrogen atomization is produced copper-Al alloy powder: add the high purity electrolytic copper in 100Kw intermediate frequency (IF) smelting stove, wait to melt back melting 15 minutes, add 15 gram copper-13% phosphorus master alloy meltings 1 minute, add copper-30% aluminium intermediate alloy melting 5 minutes again, use 0.75N/mm then 2Nitrogen atomizes, and makes-40 purpose copper-Al alloy powders;
2), oxygen source makes: get-100 order copper-Al alloy powders and be heated to 380 ℃ and be incubated 50 hours in resistance furnace, required oxygen source was made in heating in 1.5 hours under 840 ℃ of nitrogen protections then;
3), batch mixing: the oxygen source of making mixed in the V-type mixer in 1: 11 ratio with copper-Al alloy powder made powder mix in 3/4 hour;
4), isostatic cool pressing: the powder mix that mixes is packed into etc. in the static pressure gum cover, in the isostatic cool pressing Oil cylinder, be pressurized to 200N/mm then 2Moulding φ 195 * 400mm;
5), comprehensive thermal treatment: etc. the static pressure ingot under 880 ℃ of nitrogen protections, handle and in 900 ℃ of hydrogen atmospheres, reduced 5 hours after 3 hours, sintering 2 hours in 980 ℃ of hydrogen atmospheres again;
6), extruding: the powdered alloy ingot after the comprehensive thermal treatment at 850 ℃ of following extrusion molding φ 40mm alloy bar bases;
7), cold working: the excellent base of φ 40mm is cold drawn to φ 20mm, and the centre need not annealing.
7, preparation technology's method of dispersion strengthening copper alloy as claimed in claim 2, it is characterized in that: described preparation technology's method, is example to produce 110,000 high voltage isolator conducting rods with the Lcm115 alloy, and raw material adopts high purity anaerobic electrolytic copper, copper-30% aluminium intermediate alloy, copper-13% phosphorus reductor master alloy;
1), copper-aluminium dispersion strengthening copper alloy powder is produced in water atomization: add high purity anaerobic electrolytic copper in 100Kw intermediate frequency (IF) smelting stove, wait to melt back melting 15 minutes, add 15 gram copper-13% phosphorus master alloy meltings 1 minute again, add copper-30% aluminium intermediate alloy melting 5 minutes again, use 8.5N/mm then 2High pressure water-100 order copper-Al alloy powders that atomize and make;
2), oxygen source is made: get-100 order copper-Al alloy powders resistance furnace internal heating to 380 ℃ insulation 25 hours, required oxygen source was made in heating in 1.5 hours under 840 ℃ of nitrogen protections then;
3), batch mixing: the oxygen source of making and copper-Al alloy powder mixed in the V-type mixer in 1: 9 ratio made powder mix in 3/4 hour;
4), isostatic cool pressing: the powder mix that mixes packed into etc. is extruded into 200N/mm in the static pressure gum cover in the isostatic cool pressing Oil cylinder 2Moulding φ 195 * 400mm;
5), comprehensive thermal treatment: etc. after the static pressure ingot handled 3 hours under 890 ℃ of nitrogen protections, in 910 ℃ of hydrogen atmospheres, reduced 5 hours, again sintering 2 hours in 980 ℃ of hydrogen atmospheres;
6), extruding: the alloy powder ingot that comprehensive thermal treatment is finished is at the dispersion strengthening copper alloy bar of 850 ℃ of following extrusion molding φ 40mm;
7), cold working: the bar of φ 40mm carried out 75% deformation process to φ 20mm.
CN 200410029836 2004-03-30 2004-03-30 Dispersion strengthened copper alloy, and preparing technical method Expired - Fee Related CN1291049C (en)

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Cited By (21)

* Cited by examiner, † Cited by third party
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CN100417736C (en) * 2006-10-20 2008-09-10 西安理工大学 Method for preparing alumina dispersion-strenghtened copper-base composite material
CN100436634C (en) * 2005-09-30 2008-11-26 中南大学 Zero-sintering and hydrogen-expansion nano-diffusion reinforced Cu-Al2O3 alloy and its production
CN100450675C (en) * 2006-08-31 2009-01-14 昆明冶金研究院 Commercial production technique for developing alumina phase in situ in diffusive strengthened copper material
CN101914701A (en) * 2010-08-26 2010-12-15 中铝华中铜业有限公司 Lead frame material and method for processing strip made of same
CN101997103A (en) * 2009-08-19 2011-03-30 深圳市倍特力电池有限公司 Welding of battery nickel sheets
CN101178957B (en) * 2007-12-04 2011-07-27 河南科技大学 Method of producing the copper alloy contact wire
CN101178958B (en) * 2007-12-04 2011-07-27 河南科技大学 Ultra-high tension copper wire and method of producing the same
CN101708535B (en) * 2009-12-03 2012-04-18 中国船舶重工集团公司第七二五研究所 Continuously-cast crystallizer copper liner
CN102796912A (en) * 2012-08-24 2012-11-28 李艳 Preparation method of Al2O3 dispersion strengthened copper alloy bar
CN104162656A (en) * 2014-05-09 2014-11-26 苏州金江铜业有限公司 Method for preparing copper-based Al2O3 composite powder through activated carbon in-situ internal oxidation
CN104259692A (en) * 2014-10-10 2015-01-07 中铝洛阳铜业有限公司 Preparation method for car robot automatic welding station resistance welding electrode
CN104289830A (en) * 2014-10-10 2015-01-21 中铝洛阳铜业有限公司 Production method of resistance welding electrode for lithium battery connection nickel pieces
CN104976597A (en) * 2014-04-10 2015-10-14 株式会社唻迪克世 Led lamp heat radiation structure using mechanical alloying method and manufacturing method thereof
CN107574332A (en) * 2017-09-15 2018-01-12 北京有色金属研究总院 A kind of internal oxidation production alumina dispersion-strenghtened copper alloy oxidant and preparation method thereof
CN107863199A (en) * 2017-10-11 2018-03-30 陕西斯瑞新材料股份有限公司 A kind of preparation method of the copper-clad dispersion copper conducting rod of high-strength highly-conductive high softening temperature
CN107988512A (en) * 2017-11-30 2018-05-04 中铝洛阳铜加工有限公司 A kind of high strength and high flexibility cupro-nickel silicon cobalt system lead frame processing technology
CN110951988A (en) * 2019-12-18 2020-04-03 苏州金江铜业有限公司 Copper-based zirconium and zirconium oxide composite reinforced alloy and manufacturing method thereof
CN111185658A (en) * 2020-01-14 2020-05-22 广东省材料与加工研究所 Welding method of aluminum oxide copper and steel and application thereof
CN111957755A (en) * 2020-07-20 2020-11-20 华东交通大学 Drawing process for dispersion copper alloy
CN114959342A (en) * 2022-05-30 2022-08-30 河南科技大学 Method for improving processing performance of aluminum oxide dispersion strengthening copper-based composite material
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* Cited by examiner, † Cited by third party
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CN100436634C (en) * 2005-09-30 2008-11-26 中南大学 Zero-sintering and hydrogen-expansion nano-diffusion reinforced Cu-Al2O3 alloy and its production
CN100450675C (en) * 2006-08-31 2009-01-14 昆明冶金研究院 Commercial production technique for developing alumina phase in situ in diffusive strengthened copper material
CN100417736C (en) * 2006-10-20 2008-09-10 西安理工大学 Method for preparing alumina dispersion-strenghtened copper-base composite material
CN101178957B (en) * 2007-12-04 2011-07-27 河南科技大学 Method of producing the copper alloy contact wire
CN101178958B (en) * 2007-12-04 2011-07-27 河南科技大学 Ultra-high tension copper wire and method of producing the same
CN101997103A (en) * 2009-08-19 2011-03-30 深圳市倍特力电池有限公司 Welding of battery nickel sheets
CN101708535B (en) * 2009-12-03 2012-04-18 中国船舶重工集团公司第七二五研究所 Continuously-cast crystallizer copper liner
CN101914701A (en) * 2010-08-26 2010-12-15 中铝华中铜业有限公司 Lead frame material and method for processing strip made of same
CN102796912A (en) * 2012-08-24 2012-11-28 李艳 Preparation method of Al2O3 dispersion strengthened copper alloy bar
CN102796912B (en) * 2012-08-24 2014-07-16 国家电网公司 Preparation method of Al2O3 dispersion strengthened copper alloy bar
CN104976597A (en) * 2014-04-10 2015-10-14 株式会社唻迪克世 Led lamp heat radiation structure using mechanical alloying method and manufacturing method thereof
CN104162656A (en) * 2014-05-09 2014-11-26 苏州金江铜业有限公司 Method for preparing copper-based Al2O3 composite powder through activated carbon in-situ internal oxidation
CN104289830A (en) * 2014-10-10 2015-01-21 中铝洛阳铜业有限公司 Production method of resistance welding electrode for lithium battery connection nickel pieces
CN104259692A (en) * 2014-10-10 2015-01-07 中铝洛阳铜业有限公司 Preparation method for car robot automatic welding station resistance welding electrode
CN107574332A (en) * 2017-09-15 2018-01-12 北京有色金属研究总院 A kind of internal oxidation production alumina dispersion-strenghtened copper alloy oxidant and preparation method thereof
CN107863199A (en) * 2017-10-11 2018-03-30 陕西斯瑞新材料股份有限公司 A kind of preparation method of the copper-clad dispersion copper conducting rod of high-strength highly-conductive high softening temperature
CN107988512A (en) * 2017-11-30 2018-05-04 中铝洛阳铜加工有限公司 A kind of high strength and high flexibility cupro-nickel silicon cobalt system lead frame processing technology
CN110951988A (en) * 2019-12-18 2020-04-03 苏州金江铜业有限公司 Copper-based zirconium and zirconium oxide composite reinforced alloy and manufacturing method thereof
CN110951988B (en) * 2019-12-18 2021-09-21 苏州金江铜业有限公司 Copper-based zirconium and zirconium oxide composite reinforced alloy and manufacturing method thereof
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WO2024032627A1 (en) * 2022-08-09 2024-02-15 中铝洛阳铜加工有限公司 Preparation process for anti-cracking high-aluminum-content dispersion-strengthened copper electrode material

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