WO2015188378A1 - Process for preparation of high temperature, high strength and high conductivity dispersion strengthened copper alloy - Google Patents

Process for preparation of high temperature, high strength and high conductivity dispersion strengthened copper alloy Download PDF

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WO2015188378A1
WO2015188378A1 PCT/CN2014/079860 CN2014079860W WO2015188378A1 WO 2015188378 A1 WO2015188378 A1 WO 2015188378A1 CN 2014079860 W CN2014079860 W CN 2014079860W WO 2015188378 A1 WO2015188378 A1 WO 2015188378A1
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copper
powder
temperature
aluminum alloy
aluminum
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PCT/CN2014/079860
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French (fr)
Chinese (zh)
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黄劲松
刘彬
李卫
张仲灵
甘子旸
夏子航
蒋锦程
章四琪
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湖南特力新材料有限公司
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Priority to PCT/CN2014/079860 priority Critical patent/WO2015188378A1/en
Publication of WO2015188378A1 publication Critical patent/WO2015188378A1/en

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    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C1/00—Making non-ferrous alloys
    • C22C1/04—Making non-ferrous alloys by powder metallurgy
    • C22C1/05—Mixtures of metal powder with non-metallic powder
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C9/00—Alloys based on copper
    • C22C9/01—Alloys based on copper with aluminium as the next major constituent
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22F—CHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
    • C22F1/00—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
    • C22F1/08—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working of copper or alloys based thereon
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
    • H01B1/00—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors
    • H01B1/02—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors mainly consisting of metals or alloys

Definitions

  • the invention relates to a method for producing a copper-aluminum alloy.
  • dispersion strengthened copper alloy has ceramic particles (such as oxides, carbides, etc.) with high melting point, high hardness and good thermal stability and chemical inertness.
  • a type of copper alloy material formed by adding it to pure copper by in situ or ex situ methods. Compared with other reinforcement methods, Particles with dispersion strengthening do not dissolve and coarsen near the melting point of copper, nor change their mutual spacing, effectively hindering dislocation motion and grain boundary slip.
  • Dispersion-strengthened copper alloy is a metal-based composite material with excellent comprehensive physical and mechanical properties, which expands the temperature range of use of copper alloy.
  • the preparation methods of the dispersion strengthened copper alloy include an ex situ method (direct addition method) and an in situ synthesis method.
  • the direct addition method is not ideal due to various factors such as the added particles and the matrix are not coherent, and the interface strength is low.
  • In-situ recombination is a chemical reaction in-situ synthesis of strengthening phase inside a metal matrix.
  • the strengthening phase and the matrix phase are semi-coherent or even completely
  • the grid is bonded, the interface is clean and the strength is high; the reinforcing phase particles are finer and more evenly distributed.
  • In situ synthesis has incomparable advantages over non-in situ synthesized dispersion copper, and its product performance is higher.
  • the most widely used in situ synthesis method is the internal oxidation method.
  • the internal oxidation method is a method in which Al 2 O 3 is formed in situ by using oxygen in a Cu-Al alloy under selective oxygen conditions. Smith first proposed using this method to prepare dispersion-strengthened copper materials, which were later improved by Rhine and Meijering. In 1973, American SCM Company used this method for industrial production, and successively launched products such as C15715, C15720, C1572 5 and C15760.
  • the key step of the oxidation process is the oxidation of Cu-Al powder, the redox powder Cu / Al 2 O 3, pressing Cu / Al 2 O 3 reduced powder, sintered Cu / Al 2 O 3 green compact, Cu / Densification of the Al 2 O 3 alloy.
  • the pressing of the powder may be by cold isostatic pressing or molding, and the densification is usually carried out by means of cold recompression or rolling.
  • the performance of cold isostatic pressing equipment is higher than hot pressing or hot isostatic pressing, it is still lower than the molding ratio.
  • the main performance is that the molding cycle of a single blank is long, and the size of the product is also limited.
  • the object of the present invention is to provide a high-temperature, high-strength, high-conductivity dispersion-strengthened copper alloy preparation process, Increasing the density of the dispersion strengthened copper alloy to improve its electrical conductivity, increasing the size of the dispersion strengthened copper alloy ingot, achieving industrial scale production, while reducing its production cost and improving its cost performance.
  • the specific scheme of the invention is: a preparation process of a high temperature, high strength and high conductivity dispersion strengthened copper alloy, the mass percentage of aluminum is 0.15%-0.65%, the ratio of oxygen to aluminum mass is 1:1.12, and the total content of all impurities is less than 0.2%, the balance is copper, which is characterized by:
  • the copper-aluminum alloy powder used in the preparation of the dispersion strengthened copper alloy is prepared by water atomization method; the pure copper powder is fully oxidized and used as an oxidant, and the quality of the copper oxide powder is not more than 0.5% when reoxidized;
  • the prepared copper-aluminum alloy powder and the oxidizing agent CuO powder are thoroughly mixed uniformly, and the mixing time is 1-2 hours, and the ratio of the molar number of the oxidizing agent CuO powder to the molar amount of aluminum in the copper-aluminum alloy powder is (1.8-2.1):1;
  • the mixed powder is heated to 900-960 ° C in a nitrogen atmosphere having
  • the sintered alloy billet is again loaded into the steel mold, and the sintered billet is cold-repressed by means of two-way pressing on the hydraulic press, and the pressing pressure is 680-710 MPa; the cold pressed compact is annealed in a pressure sintering furnace, and the charging is performed.
  • the annealed alloy billet is again loaded into the steel mold, and the sintered billet is subjected to secondary cold recompression on the hydraulic press by means of two-way pressing, and the pressing pressure is 680-710 MPa;
  • the above-mentioned secondary cold-recompressed alloy billet is placed in a steel mold at 910-940 ° C for 120-180 min, and the steel mold is preheated at 300-450 ° C for 120-180 min, and two-way pressing is performed on the hydraulic machine.
  • the method of hot recompression of the sintered compact, the pressing pressure is 490-550 MPa.
  • the dispersion-strengthened copper alloy green body is molded by a hydraulic press, and can continuously produce large-sized ingots required for industrial production, with high efficiency and low cost.
  • the primary cold recompression of the sintered compact can increase its relative density to over 91%, and the secondary cold recompression of the cold compact after annealing at a higher temperature can increase its relative density to over 94%.
  • secondary cold recompression there are not many pores in the dispersion strengthened copper alloy, and it is basically closed pores. The friction between the surface of the dispersion strengthened copper alloy and the surface of the mold during secondary cold recompression causes the surface of the dispersion strengthened copper alloy to be completely closed.
  • the copper alloy only undergoes surface oxidation and has a good protective effect on the interior of the dispersion strengthened copper alloy.
  • the steel mold can be fully preheated at 300-450 °C to minimize the heat loss of the dispersion strengthened copper alloy during hot recompression, so that the temperature reduction is minimized, and the deformation resistance of the dispersion strengthened copper alloy at high temperature thermal deformation is fully guaranteed.
  • the degree of growth is small, and the pores are compressed or even closed during thermal recompression, and the density of the dispersion-strengthened copper alloy can approach or even reach the theoretical density.
  • the dispersion-strengthened copper alloy prepared by the process of the invention has a relative density of more than 99%, and is extruded at 930 degrees for 90 minutes, and the extrusion ratio is 14 .6
  • the tensile strength of the hot extruded alloy is greater than 550 MPa, the softening temperature is not less than 800 ° C, the relative electrical conductivity is not less than 82%, and the tensile strength is greater than 490 MPa after annealing at 900 ° C for 60 min.
  • the round bar with a diameter of 90 mm and a single mass of more than 10 kg can be continuously produced on the 5000 kN hydraulic machine by the process of the invention.
  • the invention improves the density and conductivity of the dispersion strengthened copper alloy; realizes the industrial scale production of large-sized dispersion strengthened copper alloy; reduces the production cost, and reduces the cost by more than 20% compared with the conventional internal oxidation method, thereby improving the cost performance thereof. .
  • a high temperature, high strength and high conductivity dispersion strengthened copper alloy the mass percentage of aluminum is 0.15%, and the mass percentage of oxygen is 0. .134%, the total content of all impurities is less than 0.2%, and the balance is copper.
  • the specific preparation process is as follows:
  • the pure copper powder is fully oxidized and used as an oxidizing agent, and the quality of the copper oxide powder is not more than 0.5% when reoxidized;
  • the prepared copper-aluminum alloy powder is thoroughly mixed with the oxidizing agent CuO powder, and the mixing time is 100 minutes.
  • the ratio of the number of moles of oxidant CuO powder to the number of moles of aluminum in the copper-aluminum alloy powder is 2.1:1;
  • the mixed powder is heated to 920 ° C in a nitrogen atmosphere having a purity of 99.99%, and kept for 90 minutes, and then cooled to room temperature to complete internal oxidation of the copper aluminum alloy powder;
  • the copper-aluminum alloy powder after completion of the above internal oxidation is reduced in a reducing atmosphere, the reduction temperature is 700 ° C, and the holding time is 150 min; the reduction of the internal copper oxide aluminum alloy powder is completed;
  • the reduced copper-aluminum alloy powder is placed in a steel mold, and the green body is pressed by a two-way pressing method on a hydraulic press, and the pressure is pressed.
  • the pressure is 400MPa;
  • the cold pressed green body is sintered in a pressure sintering furnace, and is filled with ordinary argon gas having a purity of 99.99%, and the pressure is 0.3 MPa.
  • the sintering temperature is 970 ° C, and the holding time is 160 min;
  • the sintered alloy billet is again loaded into the steel mold, and the sintered billet is cold-repressed by means of two-way pressing on the hydraulic press, and the pressing pressure is 690 MPa;
  • the cold pressed compact is annealed in a pressure sintering furnace and filled with ordinary argon having a purity of 99.99% at a pressure of 0.3 MPa. , annealing temperature is 680 ° C, holding time is 160 min;
  • the annealed alloy billet is again loaded into the steel mold, and the sintered billet is subjected to secondary cold recompression on the hydraulic press by means of two-way pressing, and the pressing pressure is 710 MPa;
  • the above-mentioned secondary cold-recompressed alloy billet was placed in a steel mold at 910 ° C for 120 min, and the steel mold was preheated at 450 ° C for 120 min, and the billet was heat-recovered by two-way pressing on a hydraulic press.
  • the pressing pressure was 510 MPa.
  • Example 2 The process of all of Examples 2 to 8 is similar to that of Example 1, and the process parameters are shown in Table 1 and Table 2, and are prepared in all the examples.
  • the performance indexes of the dispersion strengthened copper alloy are shown in Table 3.
  • Table 3 Properties of all examples for preparing dispersion strengthened copper alloys performance Relative density/% Tensile strength / MPa Softening temperature Relative conductivity /% After annealing strength / MPa
  • Example 1 99.1 510 850 88 496
  • Example 2 99.3 550 860 86 535
  • Example 3 99.4 585 880 84 572
  • Example 4 99.5 610 900 79 593

Abstract

A process for preparation of a high temperature, high strength and high conductivity dispersion strengthened copper alloy. The alloy contains 0.15%-0.65% of aluminum by mass percentage, and the mass ratio of oxygen to aluminum is 1:1.2. The total content of impurities is less than 0.2%, and the balance of copper. A Cu-Al alloy powder is prepared by using a water mist method. Pure copper powder is used as an oxidizing agent after being fully oxidized, and the oxidizing agent and the aluminum in the alloy powder are mixed uniformly in moles ratio (1.18-2.1):1. The mixed powder is inner-oxidized in a nitrogen atmosphere, and then reduced in a reducing atmosphere. The reduced Cu-Al alloy powder is placed into a steel mold to be pressed to a green body, and then is sintered. The sintered billet is placed into the steel mold again to be cold repressed, and then a second annealing is performed followed by a second cold repressing. Finally, the dispersion strengthened copper alloy is obtained by a hot repressing. The dispersion strengthened copper alloy prepared by the present invention has high density, good electrical conductivity, ability to be prepared in a large size, and low production cost reduced 20% or more than the traditional internal oxidation method.

Description

一种高温高强高导弥散强化铜合金制备工艺  Preparation process of high temperature, high strength and high conductivity dispersion strengthened copper alloy 技术领域 Technical field
本发明涉及一种铜铝合金的制造方法。The invention relates to a method for producing a copper-aluminum alloy.
背景技术 Background technique
弥散强化铜合金的原理是将具有高熔点、高硬度以及良好热稳定性能和化学惰性的陶瓷颗粒 (如氧化物、碳化物等 )通过原位或非原位的方法加入到纯铜中形成的一 类铜合金材料。 与其他强化方式相比, 具有弥散强化作用的粒子在接近铜熔点时不发生溶解与粗化，也不改变其相互间距，有效地阻碍位错运动与晶界滑移。弥散强化铜合金是具有优良综合物理力学性能的金属基复合材料，扩大了铜合金的使用温度范围。因为其具有较高的比强度、比模量，良好的导热性、导电性、耐磨性、高温性能，低的热膨胀系数，高的尺寸稳定性等综合性能，可以广泛应用于集成电路的引线框架，各种点焊、滚焊机的电极、触头材料，电枢、电工具的换向器，大型高速涡轮发电机的转子线，大型电气机车的架空导线等要求高电导率、高强度的元器件；也可以用于与其导电性无直接关系的热交换装置，例如连铸机结晶器内衬、电厂锅炉内喷射式点火喷孔、等离子切割枪喷嘴等，广泛应用于各个工业部门。 The principle of dispersion strengthened copper alloy is to have ceramic particles (such as oxides, carbides, etc.) with high melting point, high hardness and good thermal stability and chemical inertness. A type of copper alloy material formed by adding it to pure copper by in situ or ex situ methods. Compared with other reinforcement methods, Particles with dispersion strengthening do not dissolve and coarsen near the melting point of copper, nor change their mutual spacing, effectively hindering dislocation motion and grain boundary slip. Dispersion-strengthened copper alloy is a metal-based composite material with excellent comprehensive physical and mechanical properties, which expands the temperature range of use of copper alloy. Because of its high specific strength, specific modulus, good thermal conductivity, electrical conductivity, wear resistance, high temperature performance, low thermal expansion coefficient, high dimensional stability and other comprehensive properties, it can be widely used in the leads of integrated circuits. Frame, various spot welding, electrode of roller welder, contact material, commutator of armature, electric tool, rotor wire of large high-speed turbine generator, overhead wire of large electric locomotive, etc. require high conductivity and high strength The components can also be used for heat exchange devices that are not directly related to their conductivity, such as mold lining of continuous casting machine, jet ignition nozzle in power plant boiler, plasma cutting gun nozzle, etc., which are widely used in various industrial sectors.
弥散强化铜合金的制备方法包括非原位方法(直接外加法)和原位合成方法。直接外加法由于加入的粒子与基体不共格、界面强度低等多种因素的影响，性能不理想。原位复合法是在金属基体内部发生化学反应原位合成强化相, 与直接添加强化相粒子制取金属基复合材料相比具有如下优点：强化相与基体相之间为半共格甚至完全共格接合，界面清洁、强度高；强化相粒子更加细小且分布更加均匀。原位合成比非原位合成的弥散铜有着不可比拟的优势，产品性能更高。原位合成法研究、应用最广泛的是内氧化法。 内氧化法是利用低氧条件下Cu-Al 合金中 氧 会选择性氧化 铝 而原位生成 Al 2 O 3 的方法。 Smith 第一个提出用该方法制备弥散强化铜材料 , 后来 Rhine 和 Meijering 相继改进。 1973 年美国 SCM 公司用该法进行工业化生产 ，先后 推出了 C15715 、 C15720、 C1572 5 、 C15760 等 牌号的产品。内氧化法的关键 工序 是 Cu-Al 粉末的内氧化、 Cu / Al 2 O 3 氧化粉末的还原、 Cu / Al 2 O 3 还原粉末的压制、 Cu / Al 2 O 3 压坯 的 烧结、 Cu / Al 2 O 3 合金的致密化。 Cu-Al 粉末的内氧化、 Cu / Al 2 O 3 氧化粉末的还原和 Cu / Al 2 O 3 压坯 的 烧结，无论是研究者还是生产者，所执行的工艺参数没有很大的差别。最大的区别在于 Cu / Al 2 O 3 还原粉末的压制、 Cu / Al 2 O 3 合金的致密化这两步工序，由于压制及致密化的工艺不同，会使 Cu / Al 2 O 3 合金的生产效率与致密度产生很大的差异，从而对 Cu / Al 2 O 3 合金的性能与推广应用造成巨大的影响。将压制、烧结与热致密一次完成的方法，如在线热压或者热等静压致密的方法，虽然工艺简单，但由于设备大、能耗高、工作室小、单次毛坯的成型周期长、能生产的产品规格小，无法生产大尺寸的产品，设备的效能低(设备投资贵、使用及维护成本高)导致产品的成本高，从而大幅降低了其工业生产价值。 Cu / Al 2 O 3 合金按压制、烧结、致密化等工序依次完成时，粉末的压制可采用冷等静压或模压的方式，致密化通常采用冷复压或轧制等方式。冷等静压设备的效能虽然高于热压或热等静压的，但跟模压比还比较低，主要表现为单个毛坯的成型周期长，而产品的尺寸也受到一定的限制。要提高 弥散强化铜合金的产品尺寸，液压机模压是设备效能比、产品性价比、生产效率最高的方式，单个毛坯的成型周期也最短。但是采用 Cu-Al 粉末的内氧化、 Cu / Al 2 O 3 氧化粉末的还原、 Cu / Al 2 O 3 还原粉末的压制、 Cu / Al 2 O 3 压坯 的 烧结、 Cu / Al 2 O 3 合金的冷复压或轧制致密化的普通工艺路线所生产的 弥散强化铜合金的致密度一般为 9 6 %-99% ，很难超过99% 。从 弥散强化铜合金导电性能的影响因素可知，孔隙对其导电性能影响很大，要提高其导电性能，使其密度尽可能接近甚至达到理论密度，非常重要而且非常必要。The preparation methods of the dispersion strengthened copper alloy include an ex situ method (direct addition method) and an in situ synthesis method. The direct addition method is not ideal due to various factors such as the added particles and the matrix are not coherent, and the interface strength is low. In-situ recombination is a chemical reaction in-situ synthesis of strengthening phase inside a metal matrix. Compared with the direct addition of reinforced phase particles to obtain a metal matrix composite, it has the following advantages: the strengthening phase and the matrix phase are semi-coherent or even completely The grid is bonded, the interface is clean and the strength is high; the reinforcing phase particles are finer and more evenly distributed. In situ synthesis has incomparable advantages over non-in situ synthesized dispersion copper, and its product performance is higher. The most widely used in situ synthesis method is the internal oxidation method. The internal oxidation method is a method in which Al 2 O 3 is formed in situ by using oxygen in a Cu-Al alloy under selective oxygen conditions. Smith first proposed using this method to prepare dispersion-strengthened copper materials, which were later improved by Rhine and Meijering. In 1973, American SCM Company used this method for industrial production, and successively launched products such as C15715, C15720, C1572 5 and C15760. The key step of the oxidation process is the oxidation of Cu-Al powder, the redox powder Cu / Al 2 O 3, pressing Cu / Al 2 O 3 reduced powder, sintered Cu / Al 2 O 3 green compact, Cu / Densification of the Al 2 O 3 alloy. The internal oxidation of Cu-Al powder, the reduction of Cu / Al 2 O 3 oxidized powder and the sintering of Cu / Al 2 O 3 compact, there is no significant difference in the process parameters performed by both the researcher and the producer. The biggest difference is pressed Cu / Al 2 O 3 reduced powder, Cu / Al 2 O 3 two-step densification process of this alloy, due to the different compression and densification process, will produce Cu / Al 2 O 3 alloy There is a big difference between efficiency and density, which has a huge impact on the performance and popularization of Cu / Al 2 O 3 alloy. A method of pressing, sintering and heat densification at one time, such as on-line hot pressing or hot isostatic compaction, although the process is simple, but due to large equipment, high energy consumption, small working chamber, long molding cycle of single blank, The products that can be produced have small specifications and cannot produce large-sized products. The low efficiency of equipment (high equipment investment, high use and maintenance cost) leads to high cost of products, which greatly reduces the value of industrial production. When the pressing, sintering, densification and the like of the Cu / Al 2 O 3 alloy are sequentially completed, the pressing of the powder may be by cold isostatic pressing or molding, and the densification is usually carried out by means of cold recompression or rolling. Although the performance of cold isostatic pressing equipment is higher than hot pressing or hot isostatic pressing, it is still lower than the molding ratio. The main performance is that the molding cycle of a single blank is long, and the size of the product is also limited. To increase the product size of dispersion-strengthened copper alloys, hydraulic press molding is the most efficient way to achieve equipment efficiency, product cost performance, and productivity. The single blank has the shortest molding cycle. But using the oxidation Cu-Al powder, Cu / Al redox powder 2 O 3, pressing Cu / Al 2 O 3 reduced powder, sintered Cu / Al 2 O 3 green compact, Cu / Al 2 O 3 alloy The density of the dispersion-strengthened copper alloy produced by the ordinary process of cold recompression or rolling densification is generally from 96% to 99%, and it is difficult to exceed 99%. From the influencing factors of the conductivity of the dispersion strengthened copper alloy, it is known that the pores have a great influence on the electrical conductivity. It is very important and necessary to increase the electrical conductivity and make the density as close as possible to the theoretical density.
发明内容 Summary of the invention
本发明的目的是提供一种 高温高强高导弥散强化铜合金制备工艺， 提高弥散强化铜合金的密度以提高其导电能力，增大弥散强化铜合金锭的尺寸，实现工业化规模生产，同时降低其生产成本提高其性价比。 The object of the present invention is to provide a high-temperature, high-strength, high-conductivity dispersion-strengthened copper alloy preparation process, Increasing the density of the dispersion strengthened copper alloy to improve its electrical conductivity, increasing the size of the dispersion strengthened copper alloy ingot, achieving industrial scale production, while reducing its production cost and improving its cost performance.
本发明的具体方案为：一种高温高强高导弥散强化铜合金的制备工艺，铝的质量百分含量为0.15%-0.65%，氧与铝质量之比为1：1.12，所有杂质总含量小于0.2%，余量为铜，其特征为： 弥散强化铜合金制备所用铜铝合金粉采用水雾化法制备； 将纯铜粉充分氧化后做为氧化剂，氧化铜粉再氧化时质量增加不超过 0.5 %； 将制备的铜铝合金粉末与氧化剂CuO粉末充分混合均匀，混合时间为 1-2小时，氧化剂CuO粉末的摩尔数与铜铝合金粉末中铝的摩尔数之比为（1.8～2.1）:1 ； 将混合粉末在纯度为99.99%的氮气氛中加热到900-960℃，并保温90-150min，之后冷却至室温，完成铜铝合金粉末的内氧化； 将上述内氧化完成后的铜铝合金粉末在还原性气氛中还原，还原温度为700-760℃，保温时间为150-180min；完成内氧化铜铝合金粉末的还原； 将上述还原后的铜铝合金粉末装入钢模中 ，在液压机上采用双向压制的方式压制生坯，压制压强为340-400MPa； 将冷压制生坯在加压烧结炉中进行烧结，充入纯度 为 99.99% 的普通氩气，压力 0.3～0.5 MPa， 烧结温度为950-980℃，保温时间为120-180min； 将上述烧结合金坯再次装入钢模中，在液压机上采用双向压制的方式对烧结坯进行冷复压，压制压强为680-710MPa； 将上述冷复压坯在加压烧结炉中退火，充入纯度 为 99.99% 的普通氩气，压力 0.3～0.5MPa ，退火温度为680-710℃，保温时间为120-180min； 将上述退火后的合金坯再次装入钢模中，在液压机上采用双向压制的方式对烧结坯进行二次冷复压，压制压强为680-710MPa； 将上述二次冷复压的合金坯在910-940℃，保温120-180min后再次装入钢模中，钢模先在300-450℃预热，保温120-180min，在液压机上采用双向压制的方式对烧结坯进行热复压，压制压强为490-550MPa。 The specific scheme of the invention is: a preparation process of a high temperature, high strength and high conductivity dispersion strengthened copper alloy, the mass percentage of aluminum is 0.15%-0.65%, the ratio of oxygen to aluminum mass is 1:1.12, and the total content of all impurities is less than 0.2%, the balance is copper, which is characterized by: The copper-aluminum alloy powder used in the preparation of the dispersion strengthened copper alloy is prepared by water atomization method; the pure copper powder is fully oxidized and used as an oxidant, and the quality of the copper oxide powder is not more than 0.5% when reoxidized; The prepared copper-aluminum alloy powder and the oxidizing agent CuO powder are thoroughly mixed uniformly, and the mixing time is 1-2 hours, and the ratio of the molar number of the oxidizing agent CuO powder to the molar amount of aluminum in the copper-aluminum alloy powder is (1.8-2.1):1; The mixed powder is heated to 900-960 ° C in a nitrogen atmosphere having a purity of 99.99%, and kept for 90-150 minutes, and then cooled to room temperature to complete internal oxidation of the copper-aluminum alloy powder; The copper-aluminum alloy powder after completion of the above internal oxidation is reduced in a reducing atmosphere, the reduction temperature is 700-760 ° C, and the holding time is 150-180 min; the reduction of the internal copper oxide aluminum alloy powder is completed; The reduced copper-aluminum alloy powder is placed in a steel mold, and the green body is pressed by a two-way pressing method on a hydraulic press, and the pressing pressure is 340-400 MPa; the cold pressed green body is sintered in a pressure sintering furnace, and charged. purity 99.99% of ordinary argon, pressure 0.3-0.5 MPa, sintering temperature 950-980 ° C, holding time 120-180 min; The sintered alloy billet is again loaded into the steel mold, and the sintered billet is cold-repressed by means of two-way pressing on the hydraulic press, and the pressing pressure is 680-710 MPa; the cold pressed compact is annealed in a pressure sintering furnace, and the charging is performed. Purity 99.99% of ordinary argon, pressure 0.3 ~ 0.5MPa, annealing temperature is 680-710 ° C, holding time is 120-180min; The annealed alloy billet is again loaded into the steel mold, and the sintered billet is subjected to secondary cold recompression on the hydraulic press by means of two-way pressing, and the pressing pressure is 680-710 MPa; The above-mentioned secondary cold-recompressed alloy billet is placed in a steel mold at 910-940 ° C for 120-180 min, and the steel mold is preheated at 300-450 ° C for 120-180 min, and two-way pressing is performed on the hydraulic machine. The method of hot recompression of the sintered compact, the pressing pressure is 490-550 MPa.
本发明中 弥散强化铜合金生坯采用液压机模压，能连续生产工业化生产所需的大尺寸锭，效率高、成本低。对烧结坯的一次冷复压能将其相对密度提高到91%以上，对冷复压坯在较高的温度退火后的二次冷复压能将其相对密度提高至94%以上。通过二次冷复压，弥散强化铜合金中的孔隙已经不多，而且基本为闭孔。二次冷复压时弥散强化铜合金表面与模具表面有相互摩擦导致弥散强化铜合金表面完全封闭，这为防止弥散强化铜合金在热复压加热时的氧化打下了坚实的基础，确保弥散强化铜合金只发生表面氧化，对弥散强化铜合金的内部有良好的保护作用。钢模在300-450℃充分预热可尽量减少弥散强化铜合金在热复压时的热量损失，使其温度降低的程度尽量减少，充分保证弥散强化铜合金在高温热复变形时的变形抗力增长程度小，在热复压时孔隙被压缩甚至弥合，弥散强化铜合金的密度能接近甚至达到理论密度。 In the present invention The dispersion-strengthened copper alloy green body is molded by a hydraulic press, and can continuously produce large-sized ingots required for industrial production, with high efficiency and low cost. The primary cold recompression of the sintered compact can increase its relative density to over 91%, and the secondary cold recompression of the cold compact after annealing at a higher temperature can increase its relative density to over 94%. By secondary cold recompression, there are not many pores in the dispersion strengthened copper alloy, and it is basically closed pores. The friction between the surface of the dispersion strengthened copper alloy and the surface of the mold during secondary cold recompression causes the surface of the dispersion strengthened copper alloy to be completely closed. This lays a solid foundation for preventing the oxidation of the dispersion strengthened copper alloy during hot recompression heating, ensuring dispersion strengthening. The copper alloy only undergoes surface oxidation and has a good protective effect on the interior of the dispersion strengthened copper alloy. The steel mold can be fully preheated at 300-450 °C to minimize the heat loss of the dispersion strengthened copper alloy during hot recompression, so that the temperature reduction is minimized, and the deformation resistance of the dispersion strengthened copper alloy at high temperature thermal deformation is fully guaranteed. The degree of growth is small, and the pores are compressed or even closed during thermal recompression, and the density of the dispersion-strengthened copper alloy can approach or even reach the theoretical density.
采用本发明工艺制备的弥散强化铜合金的相对密度大于99%，将 其 在930度保温90min后挤压，挤压比为14 .6 ，热挤压态合金的抗拉强度大于550MPa，抗软化温度不小于800℃，相对电导率不小于82%，在900℃退火60min后其抗拉强度还大于490MPa。采用本发明工艺在5000kN的液压机上能连续生产直径为90mm、单根质量大于10公斤的圆棒。 本发明提高了弥散强化铜合金的密度和导电能力；实现了工业化规模地生产大尺寸的弥散强化铜合金；降低了生产成本，比传统的内氧化法降低成本20%以上，从而提高了其性价比。 The dispersion-strengthened copper alloy prepared by the process of the invention has a relative density of more than 99%, and is extruded at 930 degrees for 90 minutes, and the extrusion ratio is 14 .6 The tensile strength of the hot extruded alloy is greater than 550 MPa, the softening temperature is not less than 800 ° C, the relative electrical conductivity is not less than 82%, and the tensile strength is greater than 490 MPa after annealing at 900 ° C for 60 min. The round bar with a diameter of 90 mm and a single mass of more than 10 kg can be continuously produced on the 5000 kN hydraulic machine by the process of the invention. The invention improves the density and conductivity of the dispersion strengthened copper alloy; realizes the industrial scale production of large-sized dispersion strengthened copper alloy; reduces the production cost, and reduces the cost by more than 20% compared with the conventional internal oxidation method, thereby improving the cost performance thereof. .
具体实施方式 detailed description
实施例1  Example 1
一种高温高强高导弥散强化铜合金，铝的质量百分含量为0.15%，氧的质量百分含量为0 .134%，所有杂质总含量小于0.2%，余量为铜。具体制备工艺如下：A high temperature, high strength and high conductivity dispersion strengthened copper alloy, the mass percentage of aluminum is 0.15%, and the mass percentage of oxygen is 0. .134%, the total content of all impurities is less than 0.2%, and the balance is copper. The specific preparation process is as follows:
用水雾化法制备 铜铝合金粉 ； Preparation of copper - aluminum alloy powder by water atomization method ;
将纯铜粉充分氧化后做为氧化剂，氧化铜粉再氧化时质量增加不超过 0.5 %； The pure copper powder is fully oxidized and used as an oxidizing agent, and the quality of the copper oxide powder is not more than 0.5% when reoxidized;
将制备 的铜铝合金粉末 与氧化剂CuO粉末充分混合均匀，混合时间为100分钟， 氧化剂CuO粉末的摩尔数与铜铝合金粉末中铝的摩尔数之比为2.1:1 ； The prepared copper-aluminum alloy powder is thoroughly mixed with the oxidizing agent CuO powder, and the mixing time is 100 minutes. The ratio of the number of moles of oxidant CuO powder to the number of moles of aluminum in the copper-aluminum alloy powder is 2.1:1;
将混合粉末在纯度为99.99%的氮气氛中加热到920℃，并保温90min，之后冷却至室温，完成铜铝合金粉末的内氧化； The mixed powder is heated to 920 ° C in a nitrogen atmosphere having a purity of 99.99%, and kept for 90 minutes, and then cooled to room temperature to complete internal oxidation of the copper aluminum alloy powder;
将上述内氧化完成后的铜铝合金粉末在还原性气氛中还原，还原温度为700℃，保温时间为150min；完成内氧化铜铝合金粉末的还原； The copper-aluminum alloy powder after completion of the above internal oxidation is reduced in a reducing atmosphere, the reduction temperature is 700 ° C, and the holding time is 150 min; the reduction of the internal copper oxide aluminum alloy powder is completed;
将上述还原后的铜铝合金粉末装入钢模中 ，在液压机上采用双向压制的方式压制生坯，压 制压强为400MPa； The reduced copper-aluminum alloy powder is placed in a steel mold, and the green body is pressed by a two-way pressing method on a hydraulic press, and the pressure is pressed. The pressure is 400MPa;
将冷压制生坯在加压烧结炉中进行烧结，充入纯度 为 99.99% 的 普通氩气，压力 0.3MPa ， 烧结温度为970℃，保温时间为160min； The cold pressed green body is sintered in a pressure sintering furnace, and is filled with ordinary argon gas having a purity of 99.99%, and the pressure is 0.3 MPa. The sintering temperature is 970 ° C, and the holding time is 160 min;
将上述烧结合金坯再次装入钢模中，在液压机上采用双向压制的方式对烧结坯进行冷复压，压制压强为690MPa； The sintered alloy billet is again loaded into the steel mold, and the sintered billet is cold-repressed by means of two-way pressing on the hydraulic press, and the pressing pressure is 690 MPa;
将上述冷复压坯在加压烧结炉中退火，充入纯度 为 99.99% 的 普通氩气，压力 0.3 MPa ，退火温度为680℃，保温时间为160min； The cold pressed compact is annealed in a pressure sintering furnace and filled with ordinary argon having a purity of 99.99% at a pressure of 0.3 MPa. , annealing temperature is 680 ° C, holding time is 160 min;
将上述退火后的合金坯再次装入钢模中，在液压机上采用双向压制的方式对烧结坯进行二次冷复压，压制压强为710MPa； The annealed alloy billet is again loaded into the steel mold, and the sintered billet is subjected to secondary cold recompression on the hydraulic press by means of two-way pressing, and the pressing pressure is 710 MPa;
将上述二次冷复压的合金坯在910℃，保温120min后再次装入钢模中，钢模先在450℃预热，保温120min，在液压机上采用双向压制的方式对烧结坯进行热复压，压制压强为510MPa。 The above-mentioned secondary cold-recompressed alloy billet was placed in a steel mold at 910 ° C for 120 min, and the steel mold was preheated at 450 ° C for 120 min, and the billet was heat-recovered by two-way pressing on a hydraulic press. The pressing pressure was 510 MPa.
实施例2～实施例8 Embodiment 2 to Embodiment 8
所有实施例2～实施例8的的工艺过程同实施例1相近，工艺参数见表1和表2，所有实施例中制备 弥散强化铜合金的性能指标见表3。 The process of all of Examples 2 to 8 is similar to that of Example 1, and the process parameters are shown in Table 1 and Table 2, and are prepared in all the examples. The performance indexes of the dispersion strengthened copper alloy are shown in Table 3.
表1： 实施例1～实施例4具体工艺参数
工艺参数 实施例1 实施例2 实施例3 实施例4
弥散强化铜合金中铝含量/% 0.15 0.32 0.48 0.65
CuO 与铜铝中 Al 的摩尔比 2.1:1 1.8:1 1.9:1 2.0:1
铜铝合金粉与 CuO 粉混合时间/min 100 120 60 80
铜铝合金粉的内氧化温度/ 920 940 960 900
铜铝合金粉的内氧化时间/min 90 110 130 150
内氧化铜铝合金粉的还原温度 700 720 740 760
内氧化铜铝合金粉的还原时间 150 1 8 0 170 1 6 0
弥散强化铜生坯的压制压强 /MPa 40 0 3 8 0 3 6 0 34 0
弥散强化铜的烧结温度 970 980 950 960
弥散强化铜的烧结时间 / min 160 180 140 120
烧结弥散强化铜的冷复压压强 690 700 710 680
冷复压后的弥散强化铜的退火气氛压强 /MPa 0.3 0.4 0.5 0.4
冷复压后的弥散强化铜的退火温度 680 700 690 710
冷复压后的弥散强化铜的退火时间/min 160 140 120 180
退火后的弥散强化铜的二次冷复压压强 710 690 700 680
热复压加热温度 910 930 920 940
热复压加热时间 120 140 180 160
热复压压强 510 490 530 550
热复压钢模加热温度 450 350 400 300
热复压钢模加热时间/min 120 160 180 140
Table 1: Specific process parameters of Examples 1 to 4
Process parameters Example 1 Example 2 Example 3 Example 4
Dispersion-strengthened copper alloy aluminum content /% 0.15 0.32 0.48 0.65
Molar ratio of CuO to Al in copper and aluminum 2.1:1 1.8:1 1.9:1 2.0:1
Mixing time of copper-aluminum alloy powder with CuO powder/min 100 120 60 80
Internal oxidation temperature of copper-aluminum alloy powder / 920 940 960 900
Internal oxidation time of copper-aluminum alloy powder / min 90 110 130 150
Reduction temperature of inner copper oxide aluminum alloy powder 700 720 740 760
Reduction time of inner copper oxide aluminum alloy powder 150 1 8 0 170 1 6 0
Pressing strength of dispersion strengthened copper green body / MPa 40 0 3 8 0 3 6 0 34 0
Dispersion-strengthened copper sintering temperature 970 980 950 960
Dispersion-strengthened copper sintering time / min 160 180 140 120
Cold recompression pressure of sintered dispersion strengthened copper 690 700 710 680
Annealing atmosphere pressure of dispersion-strengthened copper after cold recompression 0.3 0.4 0.5 0.4
Annealing temperature of dispersion strengthened copper after cold recompression 680 700 690 710
Annealing time of dispersion-strengthened copper after cold recompression 160 140 120 180
Secondary cold recompression pressure of dispersion strengthened copper after annealing 710 690 700 680
Hot recompression heating temperature 910 930 920 940
Hot recompression heating time 120 140 180 160
Hot recompression pressure 510 490 530 550
Hot recompression steel mold heating temperature 450 350 400 300
Hot recompression steel mold heating time / min 120 160 180 140
表2 ：实施例5～实施例8具体工艺参数
工艺参数 实施例5 实施例6 实施例7 实施例8
弥散强化铜合金中铝含量/% 0.65 0.32 0.48 0.15
CuO 与铜铝中 Al 的摩尔比 2.1:1 2.0:1 1.8:1 1.9:1
铜铝合金粉与 CuO 粉混合时间/min 120 100 60 80
铜铝合金粉的内氧化温度/ 920 900 960 940
铜铝合金粉的内氧化时间/min 90 110 150 130
内氧化铜铝合金粉的还原温度 720 700 740 760
内氧化铜铝合金粉的还原时间 150 170 1 8 0 1 6 0
冷复压后的弥散强化铜的退火气氛压强 /MPa 0.3 0.4 0.3 0.5
弥散强化铜生坯的压制压强 /MPa 3 6 0 3 8 0 40 0 34 0
弥散强化铜的烧结温度 980 970 950 960
弥散强化铜的烧结时间 / min 140 180 160 120
烧结弥散强化铜的冷复压压强 680 700 710 690
冷复压后的弥散强化铜的退火温度 710 700 690 680
冷复压后的弥散强化铜的退火时间/min 120 140 160 180
退火后的弥散强化铜的二次冷复压压强 690 710 700 680
热复压加热温度 920 930 910 940
热复压加热时间 160 140 180 120
热复压压强 490 510 530 550
热复压钢模加热温度 350 450 400 300
热复压钢模加热时间/min 180 160 120 140
Table 2: Specific process parameters of Examples 5 to 8
Process parameters Example 5 Example 6 Example 7 Example 8
Dispersion-strengthened copper alloy aluminum content /% 0.65 0.32 0.48 0.15
Molar ratio of CuO to Al in copper and aluminum 2.1:1 2.0:1 1.8:1 1.9:1
Mixing time of copper-aluminum alloy powder with CuO powder/min 120 100 60 80
Internal oxidation temperature of copper-aluminum alloy powder / 920 900 960 940
Internal oxidation time of copper-aluminum alloy powder / min 90 110 150 130
Reduction temperature of inner copper oxide aluminum alloy powder 720 700 740 760
Reduction time of inner copper oxide aluminum alloy powder 150 170 1 8 0 1 6 0
Annealing atmosphere pressure of dispersion-strengthened copper after cold recompression 0.3 0.4 0.3 0.5
Pressing strength of dispersion strengthened copper green body / MPa 3 6 0 3 8 0 40 0 34 0
Dispersion-strengthened copper sintering temperature 980 970 950 960
Dispersion-strengthened copper sintering time / min 140 180 160 120
Cold recompression pressure of sintered dispersion strengthened copper 680 700 710 690
Annealing temperature of dispersion strengthened copper after cold recompression 710 700 690 680
Annealing time of dispersion-strengthened copper after cold recompression 120 140 160 180
Secondary cold recompression pressure of dispersion strengthened copper after annealing 690 710 700 680
Hot recompression heating temperature 920 930 910 940
Hot recompression heating time 160 140 180 120
Hot recompression pressure 490 510 530 550
Hot recompression steel mold heating temperature 350 450 400 300
Hot recompression steel mold heating time / min 180 160 120 140
表3： 所有实施例制备弥散强化铜合金的性能
性能 相对密度/% 抗拉强度/ MPa 软化温度 相对电导率 /% 退火后强度 /MPa
实施例1 99.1 510 850 88 496
实施例2 99.3 550 860 86 535
实施例3 99.4 585 880 84 572
实施例4 99.5 610 900 79 593
实施例5 99.3 615 900 78 601
实施例6 99.3 570 860 87 556
实施例7 99.3 580 875 83 565
实施例8 99.5 505 855 89 491
Table 3: Properties of all examples for preparing dispersion strengthened copper alloys
performance Relative density/% Tensile strength / MPa Softening temperature Relative conductivity /% After annealing strength / MPa
Example 1 99.1 510 850 88 496
Example 2 99.3 550 860 86 535
Example 3 99.4 585 880 84 572
Example 4 99.5 610 900 79 593
Example 5 99.3 615 900 78 601
Example 6 99.3 570 860 87 556
Example 7 99.3 580 875 83 565
Example 8 99.5 505 855 89 491

Claims (7)

  1. 一种高温高强高导弥散强化 铜合金的制 备工艺，铝的质量百分含量为0.15%-0.65%，氧与铝质量之比为1：1 .1 2，杂质总含量小于铜合金总质量的0.2%，余量为铜，其特征是：A high-temperature, high-strength, high-conductivity dispersion-strengthened copper alloy preparation process, the mass percentage of aluminum is 0.15%-0.65%, and the ratio of oxygen to aluminum mass is 1:1.1 2. The total content of impurities is less than 0.2% of the total mass of the copper alloy, and the balance is copper, which is characterized by:
    1）用水雾化法制备铜铝合金粉末；1) preparing a copper-aluminum alloy powder by water atomization;
    2）将纯铜粉充分氧化，得到氧化剂CuO粉末，氧化铜粉再氧化时质量增加不超过 0.5 %；2) The pure copper powder is sufficiently oxidized to obtain an oxidizing agent CuO powder, and the quality of the copper oxide powder is not more than 0.5% when reoxidized;
    3）将制备的铜铝合金粉末与氧化剂CuO粉末混合均匀，混合时间为1-2小时，氧化剂CuO粉末的摩尔数与铜铝合金粉末中铝的摩尔数之比为（1.8～2.1）:1；3) The prepared copper-aluminum alloy powder and the oxidant CuO powder are uniformly mixed for a mixing time of 1-2 hours, and the ratio of the mole number of the oxidizing agent CuO powder to the number of moles of aluminum in the copper-aluminum alloy powder is (1.8 to 2.1): ;
    4）将混合粉末在纯度为99.99%的氮气氛中加热到900-960℃，并保温90-150min，之后冷却至室温，完成铜铝合金粉末的内氧化；4) heating the mixed powder to 900-960 ° C in a nitrogen atmosphere having a purity of 99.99%, and maintaining the temperature for 90-150 minutes, and then cooling to room temperature to complete internal oxidation of the copper-aluminum alloy powder;
    5）将上述内氧化完成后的铜铝合金粉末在还原性气氛中还原，还原温度为700-760℃，保温时间为150-180min；完成内氧化铜铝合金粉末的还原；5) reducing the copper-aluminum alloy powder after completion of the above internal oxidation in a reducing atmosphere, the reduction temperature is 700-760 ° C, and the holding time is 150-180 min; the reduction of the internal copper oxide aluminum alloy powder is completed;
    6）将上述还原后的铜铝合金粉末装入钢模中，在液压机上采用双向压制的方式压制生坯，压制压强为340-400MPa；6) The above-mentioned reduced copper-aluminum alloy powder is charged into a steel mold, and the green body is pressed by a two-way pressing method on a hydraulic press, and the pressing pressure is 340-400 MPa;
    7）将冷压制生坯在加压烧结炉中进行烧结，充入纯度为 99.99% 的普通氩气，压力 0.3～0.5MPa ，烧结温度为950-980℃，保温时间为120-180min；7) The cold pressed green body is sintered in a pressure sintering furnace, and is filled with ordinary argon gas having a purity of 99.99%, and the pressure is 0.3 to 0.5 MPa. , sintering temperature is 950-980 ° C, holding time is 120-180 min;
    8）将烧结铜铝合金坯再次装入钢模中，在液压机上采用双向压制的方式对烧结坯进行冷复压，压制压强为680-710MPa；8) The sintered copper-aluminum alloy billet is again loaded into the steel mold, and the sintered billet is cold-repressed by means of two-way pressing on the hydraulic press, and the pressing pressure is 680-710 MPa;
    9)将冷复压后的铜铝合金坯在加压烧结炉中退火，充入纯度为 99.99% 的普通氩气，压力 0.3 ～0.5 MPa ，退火温度为680-710℃，保温时间为120-180min；9) Annealing the cold-recompressed copper-aluminum alloy billet in a pressure sintering furnace, charging a normal argon gas with a purity of 99.99%, and a pressure of 0.3 to 0.5 MPa. , annealing temperature is 680-710 ° C, holding time is 120-180 min;
    10)将退火后的铜铝合金坯再次装入钢模中，在液压机上采用双向压制的方式对烧结坯进行二次冷复压，压制压强为680-710MPa；10) The annealed copper aluminum alloy billet is again loaded into the steel mold, and the sintered billet is subjected to secondary cold recompression on the hydraulic press by means of two-way pressing, and the pressing pressure is 680-710 MPa;
    11)将二次冷复压的铜铝合金坯在910-940℃，保温120-180min后再次装入钢模中，钢模先在300-450℃预热，保温120-180min，在液压机上采用双向压制的方式对烧结坯进行热复压，压制压强为490-550MPa。11) The secondary cold-recompressed copper-aluminum alloy billet is placed in the steel mold at 910-940 ° C for 120-180 min. The steel mold is preheated at 300-450 ° C for 120-180 min, on a hydraulic press. The sintered compact is hot-repressed by means of two-way pressing, and the pressing pressure is 490-550 MPa.
  2. 如权利要求1所述的一种高温高强高导弥散强化 铜合金的制 备工艺，其特征在于：氧化剂CuO粉末的摩尔数与铜铝合金粉末中铝的摩尔数之比为（1.9～2.1）:1。A high temperature, high strength, high permeability, dispersion strengthened copper alloy according to claim 1 The preparation process is characterized in that the ratio of the number of moles of the oxidizing agent CuO powder to the number of moles of aluminum in the copper-aluminum alloy powder is (1.9 to 2.1):1.
  3. 如权利要求2所述的一种高温高强高导弥散强化 铜合金的制 备工艺，其特征在于：氧化剂CuO粉末的摩尔数与铜铝合金粉末中铝的摩尔数之比为（2.0～2.1）:1。A high temperature, high strength, high permeability, dispersion strengthened copper alloy according to claim 2 The preparation process is characterized in that the ratio of the number of moles of the oxidizing agent CuO powder to the number of moles of aluminum in the copper-aluminum alloy powder is (2.0 to 2.1):1.
  4. 如权利要求1所述的一种高温高强高导弥散强化 铜合金的制 备工艺，其特征在于：步骤4）所述的氮气氛中加热的温度为910-950℃。A high temperature, high strength, high permeability, dispersion strengthened copper alloy according to claim 1 The preparation process is characterized in that the temperature of heating in the nitrogen atmosphere described in the step 4) is 910-950 °C.
  5. 如权利要求4所述的一种高温高强高导弥散强化 铜合金的制 备工艺，其特征在于：步骤4）所述的氮气氛中加热的温度为920-950℃。 A high temperature, high strength, high permeability, dispersion strengthened copper alloy according to claim 4 The preparation process is characterized in that the temperature of heating in the nitrogen atmosphere described in the step 4) is 920-950 °C.
  6. 如权利要求1所述的一种高温高强高导弥散强化 铜合金的制 备工艺，其特征在于：步骤5）所述的还原温度为710-750℃。A high temperature, high strength, high permeability, dispersion strengthened copper alloy according to claim 1 The preparation process is characterized in that the reduction temperature in the step 5) is 710-750 °C.
  7. 如权利要求6所述的一种高温高强高导弥散强化 铜合金的制 备工艺，其特征在于：步骤5）所述的还原温度为710-740℃。 A process for preparing a high temperature, high strength, high permeability, dispersion strengthened copper alloy according to claim 6, wherein the reduction temperature in the step 5) is 710 to 740 °C.
PCT/CN2014/079860 2014-06-13 2014-06-13 Process for preparation of high temperature, high strength and high conductivity dispersion strengthened copper alloy WO2015188378A1 (en)

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CN108251671A (en) * 2018-01-08 2018-07-06 北京科技大学 A kind of preparation method for adulterating graphene oxide enhancing ODS copper
CN108856725A (en) * 2018-06-13 2018-11-23 东南大学 A kind of preparation method and application of dispersion-strengthened Cu in situ composites
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CN111687424A (en) * 2020-05-19 2020-09-22 陕西斯瑞新材料股份有限公司 Preparation method and application of copper-iron alloy powder
CN114632934A (en) * 2022-02-17 2022-06-17 贵州新安航空机械有限责任公司 Double-layer copper alloy powder metallurgy pantograph slide plate and manufacturing process thereof
CN114807673A (en) * 2022-05-23 2022-07-29 安徽富悦达电子有限公司 Alloy material for high-strength high-conductivity wire harness terminal and preparation method thereof
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
CN115488335A (en) * 2022-09-28 2022-12-20 陕西斯瑞新材料股份有限公司 Manufacturing method of copper-chromium contact material for high voltage grade

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CN105714140A (en) * 2016-02-29 2016-06-29 苏州莱特复合材料有限公司 Copper base alloy material and preparation method thereof
CN108251671A (en) * 2018-01-08 2018-07-06 北京科技大学 A kind of preparation method for adulterating graphene oxide enhancing ODS copper
CN108856725A (en) * 2018-06-13 2018-11-23 东南大学 A kind of preparation method and application of dispersion-strengthened Cu in situ composites
CN110625126A (en) * 2019-10-14 2019-12-31 中铝洛阳铜加工有限公司 Preparation method of high-conductivity high-heat-resistance dispersion oxygen-free copper
CN111687424B (en) * 2020-05-19 2023-09-08 陕西斯瑞新材料股份有限公司 Preparation method and application of copper-iron alloy powder
CN111687424A (en) * 2020-05-19 2020-09-22 陕西斯瑞新材料股份有限公司 Preparation method and application of copper-iron alloy powder
CN114632934A (en) * 2022-02-17 2022-06-17 贵州新安航空机械有限责任公司 Double-layer copper alloy powder metallurgy pantograph slide plate and manufacturing process thereof
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CN114807673A (en) * 2022-05-23 2022-07-29 安徽富悦达电子有限公司 Alloy material for high-strength high-conductivity wire harness terminal and preparation method thereof
CN114807673B (en) * 2022-05-23 2023-10-10 安徽富悦达电子有限公司 Alloy material for high-strength high-conductivity wire harness terminal and preparation method thereof
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
CN114959342B (en) * 2022-05-30 2024-03-29 河南科技大学 Method for improving processability of aluminum oxide dispersion strengthening copper-based composite material
CN115488335B (en) * 2022-09-28 2023-07-25 陕西斯瑞新材料股份有限公司 Manufacturing method of copper-chromium contact material for high voltage level
CN115488335A (en) * 2022-09-28 2022-12-20 陕西斯瑞新材料股份有限公司 Manufacturing method of copper-chromium contact material for high voltage grade

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