CN1905082A - High strength high conducting copper-rare-earth alloy material and preparing process thereof - Google Patents
High strength high conducting copper-rare-earth alloy material and preparing process thereof Download PDFInfo
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- CN1905082A CN1905082A CN 200610019238 CN200610019238A CN1905082A CN 1905082 A CN1905082 A CN 1905082A CN 200610019238 CN200610019238 CN 200610019238 CN 200610019238 A CN200610019238 A CN 200610019238A CN 1905082 A CN1905082 A CN 1905082A
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- 229910052802 copper Inorganic materials 0.000 claims abstract description 22
- 238000002360 preparation method Methods 0.000 claims abstract description 22
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- QEFYFXOXNSNQGX-UHFFFAOYSA-N neodymium atom Chemical compound [Nd] QEFYFXOXNSNQGX-UHFFFAOYSA-N 0.000 claims abstract description 6
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Abstract
本发明公开了一种高强高导电铜－稀土合金材料及其制备工艺，合金各成分的按质量比为：铜∶铬∶钕为97.6－98.8∶0.4－1.1∶0.02－0.08。本发明制备工艺包括合金的熔铸工艺、合金熔铸后的处理工艺，合金熔铸后的处理工艺中直接对合金铸锭冷轧，再进行时效处理。本发明所述制备工艺在合金熔铸时，直接添加纯金属Cr颗粒，浇铸温度为1100℃－1250℃。本发明合金材料具有以下特点：抗拉强度为470－510MPa，延伸率为12－15％，导电率为88－91％IACS，软化温度为510－540℃。本发明合金的熔铸技术不仅简化工艺，减少偏析，而且有利于合金成分的精确控制。本发明合金制备工艺简单，性能优异，可广泛适用于电子工业和机械行业等要求高导高强以及较高工作温度下使用的场合，尤其适用于要求高强高导及良好加工性能的微电子行业。
The invention discloses a high-strength and high-conductivity copper-rare earth alloy material and its preparation process. The mass ratio of the components of the alloy is: copper: chromium: neodymium is 97.6-98.8: 0.4-1.1: 0.02-0.08. The preparation process of the invention includes alloy melting and casting process, alloy casting process and alloy casting process. In the alloy casting process, alloy casting ingots are directly cold-rolled and then subjected to aging treatment. The preparation process of the present invention directly adds pure metal Cr particles when the alloy is melted and casted, and the casting temperature is 1100°C-1250°C. The alloy material of the invention has the following characteristics: the tensile strength is 470-510 MPa, the elongation is 12-15%, the electrical conductivity is 88-91% IACS, and the softening temperature is 510-540 DEG C. The melting and casting technology of the alloy of the invention not only simplifies the process and reduces segregation, but also facilitates the precise control of the alloy composition. The alloy of the invention has a simple preparation process and excellent performance, and can be widely used in the electronic industry and machinery industry where high conductivity, high strength and high working temperature are required, and is especially suitable for the microelectronic industry that requires high strength, high conductivity and good processing performance.
Description
Technical field:
The invention belongs to metal electron material field, relate to a kind of high-strength high-conductivity copper-rare-earth alloy material and preparation technology, relate in particular to a kind of high-intensity high-conductivity copper chromium neodymium alloy and preparation technology thereof.
Background technology:
Development, exploitation high-intensity high-conductivity copper base conductive material are one of focuses of copper alloy research always.Many applications require material therefor to need high conductance and high strength to have both.According to different structures and performance characteristics, the high-intensity high-conductivity copper sill can be divided into copper alloy with high strength and high conductivity and high-strength highly-conductive Cu-base composites two big classes.Two class materials all are not quite similar at aspects such as strengthening mechanism, preparation technology, performance characteristics and even applications.In recent years, fully utilize various intensifying methods, the performance of high-intensity high-conductivity copper sill is greatly improved.
Solution strengthening, working hardening, intercrystalline strengthening, precipitation strength, complex intensifying are five kinds of main reinforcement means when design high-strength highly-conductive copper-based material, and its essence all is that motion by stoping dislocation is with strengthening material.Preceding four kinds of reinforcement means apply to the reinforcement of copper alloy usually, and complex intensifying is mainly used in the reinforcement of Cu-base composites.Present high performance high-strength highly-conductive copper-based material often fully utilizes various strengthening mechanisms to improve performance to greatest extent, reduces cost.Because alloying element can have a strong impact on copper matrix electric conductivity when existing with the solid solution attitude, when the design copper alloy with high strength and high conductivity, rule or in the copper matrix, have low-down solid solubility (Cr when requiring selected alloying element room temperature, Zr, Fe, Ag, Be etc.), or can form compound precipitation (Fe between alloying element
2P, Cu
3Zr, Mg
mP
n, Ni
2Si etc.).In addition, can add some auxiliary elements favourable, (prevent from fragility Cu mutually to occur between metallic matrix and coating as P (deoxidation, prevent hydrogen embrittlement), Zn to alloy property
3Sn, Cu
5Sn
6) and Mg (improving material stress relaxation-resistant characteristic) etc.
For high-strength highly-conductive deformation copper-based material, not only require alloying element and copper at room temperature to have low-down mutual solubility, the second phase constituent element also will have good plasticity simultaneously, to prevent wild phase and basal body interface cracking when carrying out large deformation.According to analysis to a large amount of copper alloy binary phase diagramls, have only Cu-Ag, Cu-bcc (Nb, Ta, Fe, V, Cr is to satisfy above-mentioned requirements Mo).
The typical preparation technology of precipitation strength type copper alloy is: melting and casting-homogenizing processing-hot rolling-solution treatment-cold rolling-timeliness.Lead the melting and the casting of high-strength copper alloy for height, mainly pay attention to the optimization of melting and pouring technology,, and reduce the melting cost as far as possible with the acquisition mother alloy ingot that casting flaw is few, composition is even, impurity content is little.After adopting casting to prepare mother alloy ingot, handle the component segregation that causes in the casting process to eliminate through homogenizing; Subsequently ingot casting is carried out the predeformation hot rolling, and eliminate thick, the heterogeneous structure that forms in casting and the homogenizing process by dynamic recrystallization.The hot rolling sample carries out solution treatment in certain temperature, carries out Ageing Treatment after handling through cold deformation to a certain degree.Cold deformation can be introduced a large amount of point, line defect in alloy substrate, these defectives can be quickened precipitation process and refinement precipitated phase particle as the forming core core of precipitated phase in the ag(e)ing process and the diffusion admittance of atom.To precipitation strength type copper alloy with high strength and high conductivity, alloy property depends on the kind of precipitated phase, with the deflection of basal body interface bond type, quantity, shape, size, distribution and alloy etc.Big predeformation, timeliness can obtain the highest hardness and higher conductance in short-term.Because the peculiar property that rare earth element had often is added on it and carries out modification in metal material as micro alloying element, the interpolation of a small amount of rare earth can change alloy organizing structure, impurity content, state of interface etc., finally influences the performance of alloy.This influence both may be useful, also may be harmful to, and depended on alloy system kind and all kinds of process conditions.Forefathers mainly concentrate on the following aspects to the research work of rare earth action effect in metal material: the purification of rare earth, rotten, microalloying effect and to the influence of material conductivity, processing and mechanical property, resistance to wear, non-oxidizability etc.Rare earth has obtained using widely in iron and steel, aluminium at present, has grasped great deal of experiment data, and its action effect and mechanism have been carried out deep research.The utilization of rare earth in copper alloy still put into practice all and can not be compared with the above two in theory.
The circuit lead frame material is important use field of copper alloy with high strength and high conductivity, accounted at present more than 80% of blaster fuse frame material consumption, develop the high, medium and low shelves copper alloy for lead-wire frame series of more than the 100 kind of trade mark, table 1 has been listed the main performance of part copper alloy lead wire frame material.China is in the scientific research of lead frame Cu alloy material and produce and all lag behind advanced country, and the production kind is few, yield poorly the basic dependence on import of particularly senior blaster fuse frame material.Though some blaster fuse frame material production and processing enterprises have been arranged at present, by imitated and technology transfer, the product with independent intellectual property right have been arranged seldom substantially.More existing scientific research institutions, universities and colleges carry out the development of this type of material, as Tsing-Hua University, Luoyang Polytechnical College, University Of Nanchang etc., but are in laboratory stage substantially, can not satisfy the needs of China's microelectronic industry fast development at all.Therefore, develop as early as possible at present that the novel high-strength height is led and the copper base blaster fuse frame material of high softening temperature has become the task of top priority, have great importance.
Lead frame alloy and performance that table 1 is commonly used
| Alloy designations | Chemical composition (wt%) | Tensile strength MPa | Elongation (%) | Conductance %IACS | Softening temperature ℃ |
| C19400 (day) | Cu-2.35Fe-0.12Zn-0.03P | 362～568 | 4～5 | 55～65 | ---- |
| OMCL-1 (day) | Cu-0.3Cr-0.1Zr-0.05Mg | 590 | 8 | 82 | ---- |
| KLF-125 (day) | Cu-3.2Ni-0.7Si-1.25Sn-0.3Zn | 667 | 9 | 35 | ---- |
| Alloy 42 (day) TFe0.1 QFe2.5 QSi0.25 JK-2 | 42Ni-58Fe Cu-0.1Fe-0.03P Cu-2.5Fe-0.05Zn-0.03P Cu-1.0Ni-0.25Si-0.1Zn Ni＜2, Sn＜1.5 CuCrZrZn system | 650 335～410 365～441 550 608 525 | --- 4～5 5～6 ≥6 6 ---- | 2.7 ＞80 ＞60 61 32 80 | 320 400 440 400 ---- ---- |
Summary of the invention:
The object of the invention is to provide a kind of new copper alloy with high strength and high conductivity material, under sufficiently high intensity, still keep up to the conductance of 88-91%IACS and the elongation of 12-15%, both having can be used as requirement has the blaster fuse frame material of excellent machinability, again applicable to microelectronics that requires high-strength highly-conductive and power industry.
For achieving the above object, copper provided by the invention-rare earth alloy technical scheme is as follows:
Each composition of alloy of the present invention by mass ratio be: copper: chromium: neodymium is 97.6-98.8: 0.4-1.1: 0.02-0.08.
The preparation technology of high strength high conducting copper-rare-earth alloy material of the present invention comprises the founding of alloy, the treatment process behind the alloy casting, and is directly cold rolling to alloy cast ingot in the treatment process behind the alloy casting, carries out Ageing Treatment again.
Preparation technology of the present invention directly adds simple metal Cr particle when alloy casting, cast temperature is 1100 ℃-1250 ℃.
During preparation technology's alloy casting of the present invention, adopt the Cu-Nd intermediate alloy, the Nd content in the intermediate alloy is 7-18wt%, and adds the Cu-Cr alloy of molten state.
Preparation technology of the present invention is after cold rolling, and the temperature of carrying out Ageing Treatment is 380 ℃-600 ℃.
Preparation technology of the present invention is 99.7-99.9wt% in the Metal Cr particle purity of adding, and granular size is 0.5-3.0mm.
Keep during preparation technology's founding of the present invention that vacuum degree is 2 * 10 in the stove
-1Pa-1 * 10
-2Pa.
Specifying of alloy technology scheme of the present invention is as follows:
1. the founding of alloy
A) .Cu-Nd (Nd:7-18wt%) intermediate alloy founding
Frequently first melting copper in the induction furnace in a vacuum, the rare earth metal Nd fragment of additional proportion composition then, it is standby to be cast into bar in 1100 ℃～1300 ℃.
B) .Cu-Cr-Nd alloy casting
First melting copper in the frequency induction furnace then directly adds the Cr particle in a vacuum, treats to add the Cu-Nd intermediate alloy after the fusion, and holding temperature is 1200 ℃-1350 ℃, and cast temperature is 1100 ℃-1250 ℃, and keeping the interior vacuum degree of stove is 2 * 10
-1Pa-1 * 10
-2Pa.
2. the treatment process behind the alloy casting
Alloy cast ingot after the casting directly carries out cold rollingly after surface peeling without solution treatment, carry out Ageing Treatment at 380 ℃-600 ℃ then, and temperature retention time 30min-60min takes out with stove cooling back.
Alloy material of the present invention has following characteristics: tensile strength is 470-510MPa, and elongation is 12-15%, and conductance is 88-91%IACS, and softening temperature is 510-540 ℃.The casting technology of alloy of the present invention is not only simplified technology, reduces segregation, and helps the accurate control of alloying component.Processing and processing technology behind the alloy casting have further shortened the production cycle, have saved cost.Alloy preparation technology of the present invention is simple, and excellent performance can be widely used in that requirements such as electronics industry and mechanical industry are high to be led high-strength and than the occasion that elevated operating temperature uses down, be particularly useful for the microelectronic industry of requirement high-strength highly-conductive and excellent machinability.
Description of drawings
Fig. 1: the Cr element is along the vertical distribution map of Cu-Cr-Nd ingot casting
Fig. 2: the different process flow process is to the influence of alloy rigidity
Fig. 3: the different process flow process is to the influence of alloy conductivity
Embodiment
The present invention is described in detail below in conjunction with embodiment.
Embodiment 1:
It is that 99.9% cathode copper, purity are that 99.9% electrolysis chromium, purity are 99.5% rare earth metal neodymium that raw material adopt purity.Carry out the melting of Cu-Nd (Nd:8wt%) intermediate alloy earlier, method is a first melting copper in the induction furnace frequently in a vacuum, the rare earth metal Nd fragment of additional proportion composition then, and it is standby to be cast into bar in 1150 ℃.Then by Cu: the mass ratio of Cr: Nd is to carry out the Cu-Cr-Nd alloy melting at 98.20: 0.70: 0.03, frequently first melting copper in the induction furnace in a vacuum, then directly add and pulverize the pure Cr particle in back, granular size is 0.5-1.0mm, treat to add the Cu-Nd intermediate alloy after the fusion, holding temperature is 1300 ℃, and cast temperature is 1180 ℃, and keeping the interior vacuum degree of stove is 1.5 * 10
-2Pa, the casting rod that is cast into.Cut the casting rod end to end, surface finish is smooth, direct cold rolling, the accumulation drafts is about 95%.Under vacuum, carry out Ageing Treatment, 430 ℃ of aging temps, temperature retention time 35min takes out with stove cooling back.The 98.20Cu-0.70Cr-0.05Nd alloy conductive rate that obtains through above-mentioned technology reaches 90%IACS, and hot strength reaches 510MPa, and softening temperature reaches 540 ℃.
Embodiment 2:
It is that 99.9% cathode copper, purity are that 99.9% electrolysis chromium, purity are 99.5% rare earth metal neodymium that raw material adopt purity.Carry out the melting of Cu-Nd (Nd:9wt%) intermediate alloy earlier, method is a first melting copper in the induction furnace frequently in a vacuum, the rare earth metal Nd fragment of additional proportion composition then, and it is standby to be cast into bar in 1100 ℃.Then by Cu: the mass ratio of Cr: Nd is to carry out the Cu-Cr-Nd alloy melting at 98.20: 0.90: 0.04, frequently first melting copper in the induction furnace in a vacuum, then directly add the pure Cr particle after pulverizing, granular size is 1.8-2.5mm, treat to add the Cu-Nd intermediate alloy after the fusion, holding temperature is 1250 ℃, and cast temperature is 1100 ℃, and keeping the interior vacuum degree of stove is 1 * 10
-2Pa, the casting rod that is cast into.Cut the casting rod end to end, surface finish is smooth, direct cold rolling, the accumulation drafts is about 95%.Under vacuum, carry out Ageing Treatment, 500 ℃ of aging temps, temperature retention time 30min takes out with stove cooling back.The 98.20Cu-0.90Cr-0.04Nd alloy conductive rate that obtains through above-mentioned technology reaches 91%IACS, and hot strength reaches 500MPa, and softening temperature reaches 530 ℃.
Embodiment 3:
It is that 99.9% cathode copper, purity are that 99.9% electrolysis chromium, purity are 99.5% rare earth metal neodymium that raw material adopt purity.Carry out the melting of Cu-Nd (Nd:12wt%) intermediate alloy earlier, method is a first melting copper in the induction furnace frequently in a vacuum, the rare earth metal Nd fragment of additional proportion composition then, and it is standby to be cast into bar in 1200 ℃.Then by Cu: the mass ratio of Cr: Nd is to carry out the Cu-Cr-Nd alloy melting at 98.2: 0.9: 0.06, frequently first melting copper in the induction furnace in a vacuum, then directly add and pulverize the pure Cr particle in back, granular size is 2.0-3.0mm, treat to add the Cu-Nd intermediate alloy after the fusion, holding temperature is 1200 ℃, and cast temperature is 1100 ℃, and keeping the interior vacuum degree of stove is 2 * 10
-2Pa, the casting rod that is cast into.Cut the casting rod end to end, surface finish is smooth, direct cold rolling, the accumulation drafts is about 95%.Under vacuum, carry out Ageing Treatment, 380 ℃ of aging temps, temperature retention time 40min takes out with stove cooling back.The 98.2Cu-0.9Cr-0.06Nd alloy conductive rate that obtains through above-mentioned technology reaches 88%IACS, and hot strength reaches 490MPa, and softening temperature reaches 520 ℃.
Know-why of the present invention relates to:
A). low chromium-copper evanohm (containing chromium 0.4-1.2wt%) founding: according to copper chromium binary phase diagraml as can be known, the chromiumcopper eutectic composition is about 1.28wt%.When the hypereutectic alloy cooling procedure enters Mushy Zone by liquid phase region, at first separate out nascent Cr, because Cr proportion is less than Cu, easily come-up causes gravity segregation, chromium content is high more, segregation is serious more, and prepared intermediate alloy uneven components can't accurately be controlled composition when causing later alloy casting.But alloying component of the present invention contains chromium less than 1.28wt%, is hypoeutectic alloy, and its temperature interval and composition are at interval all much smaller than hypereutectic alloy, and the flowability when therefore solidifying is better, and the segregation after solidifying also can be littler.The present invention adopts the melting technique of the pure chromium of direct interpolation for this reason, can obtain near nominal composition after the founding and does not have the Cu-Cr-Nd alloy-steel casting of gross segregation.Fig. 1 is the Cr element that obtains through the glow discharge spectrometry constituent analysis along ingot casting distribution map longitudinally, shows that the ingot casting with this technology casting does not almost have gross segregation.
B). cold deformation and timeliness are handled: cold deformation can be introduced a large amount of point, line defect in alloy substrate, these defectives can improve the intensity of alloy on the one hand, can quicken precipitation process and refinement precipitated phase particle as the forming core core of precipitated phase in the ag(e)ing process and the diffusion admittance of atom on the other hand.Nonferrous materials will be implemented homogenizing usually and handle after founding, will pass through solution treatment usually before the cold deformation, the purpose of precipitating reinforcing effect when reaching Ageing Treatment after solution strengthening and the raising cold deformation.Alloy of the present invention is handled admittedly need not homogenizing owing to can obtain non-segregationalloy when founding; When considering alloy casting of the present invention again and nonequilibrium freezing, alloy element effectively dissolves in matrix, therefore also can save solid solution treatment process, directly carries out cold deformation and Ageing Treatment.From Fig. 2 as seen through 95% the alloy after cold rolling not as other alloy ag(e)ing process hardness obviously descend, illustrate its reply and again crystallization rate be lower than solid solution+cold rolling+aging alloy, this may be because the quench cooling rate of alloy when cooling rate is lower than solution treatment in being cast into the process of ingot casting, the supersaturation room that this relatively low cooling rate keeps in matrix is less, and the existence in these rooms can promote to reply and the carrying out of crystallization again.Reply on the other hand and again crystallization reduced point defect density again, make the conductivity of alloy increase to some extent, and effect is than adopting the more obvious (see figure 3) of alloy that solid solution+cold rolling+the timeliness mode is handled.
Claims (7)
1, a kind of high strength high conducting copper-rare-earth alloy material is characterized in that: each composition of alloy by mass ratio be: copper: chromium: neodymium is 97.6-98.8: 0.4-1.1: 0.02-0.08.
2, a kind of preparation technology by the described high strength high conducting copper-rare-earth alloy material of claim 1, comprise the founding of alloy, the treatment process behind the alloy casting, it is characterized in that: directly cold rolling in the treatment process behind the alloy casting to alloy cast ingot, carry out Ageing Treatment again.
3, a kind of preparation technology by the described high strength high conducting copper-rare-earth alloy material of claim 2, it is characterized in that: during alloy casting, directly add simple metal Cr particle, cast temperature is 1100 ℃-1250 ℃.
4, press the preparation technology of claim 2 and the described high strength high conducting copper-rare-earth alloy material of claim 3, it is characterized in that: during alloy casting, adopt the Cu-Nd intermediate alloy, the Nd content in the intermediate alloy is 7-18wt%, and adds the Cu-Cr alloy of molten state.
5, by the preparation technology of claim 2 and the described high strength high conducting copper-rare-earth alloy material of claim 3, it is characterized in that: after cold rolling, the temperature of carrying out Ageing Treatment is 380 ℃-600 ℃.
6, by the preparation technology of the described high strength high conducting copper-rare-earth alloy material of claim 3, it is characterized in that: the Metal Cr particle purity of interpolation is 99.7-99.9wt%, and granular size is 0.5-3.0mm.
7, by the preparation technology of claim 2 and the described high strength high conducting copper-rare-earth alloy material of claim 3, it is characterized in that: keeping the interior vacuum degree of stove during founding is 2 * 10
-1Pa-1 * 10
-2Pa.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101768680B (en) * | 2008-12-26 | 2011-07-20 | 北京有色金属研究总院 | Composite modifier for copper alloy of lead frame |
| CN103088225A (en) * | 2012-12-21 | 2013-05-08 | 江苏中容铜业有限公司 | Preparation method of oxygen-free copper base alloy for propeller |
| CN103911572A (en) * | 2014-04-04 | 2014-07-09 | 江苏藤仓亨通光电有限公司 | Production technique of high-strength high-conductivity copper alloy contact network line |
| CN106381414A (en) * | 2016-09-30 | 2017-02-08 | 陕西科技大学 | Copper-based in-situ composite alloy and preparing method thereof |
| CN114032414A (en) * | 2021-11-17 | 2022-02-11 | 湖南稀土金属材料研究院有限责任公司 | Modified copper-chromium alloy and preparation method and application thereof |
| CN116397128A (en) * | 2023-04-18 | 2023-07-07 | 中国科学院金属研究所 | Rare earth copper chromium alloy material and preparation method thereof |
Family Cites Families (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2000234151A (en) * | 1998-12-15 | 2000-08-29 | Shin Etsu Chem Co Ltd | R-Fe-B rare earth permanent magnet material |
| CN1254554C (en) * | 2002-11-15 | 2006-05-03 | 清华大学 | High-strength and high-conductivity RE-Cu alloy and its production process |
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2006
- 2006-05-30 CN CNB2006100192384A patent/CN100433198C/en not_active Expired - Fee Related
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101768680B (en) * | 2008-12-26 | 2011-07-20 | 北京有色金属研究总院 | Composite modifier for copper alloy of lead frame |
| CN103088225A (en) * | 2012-12-21 | 2013-05-08 | 江苏中容铜业有限公司 | Preparation method of oxygen-free copper base alloy for propeller |
| CN103911572A (en) * | 2014-04-04 | 2014-07-09 | 江苏藤仓亨通光电有限公司 | Production technique of high-strength high-conductivity copper alloy contact network line |
| CN103911572B (en) * | 2014-04-04 | 2016-07-06 | 江苏藤仓亨通光电有限公司 | A kind of production technology of copper alloy with high strength and high conductivity contact net lines |
| CN106381414A (en) * | 2016-09-30 | 2017-02-08 | 陕西科技大学 | Copper-based in-situ composite alloy and preparing method thereof |
| CN114032414A (en) * | 2021-11-17 | 2022-02-11 | 湖南稀土金属材料研究院有限责任公司 | Modified copper-chromium alloy and preparation method and application thereof |
| CN116397128A (en) * | 2023-04-18 | 2023-07-07 | 中国科学院金属研究所 | Rare earth copper chromium alloy material and preparation method thereof |
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| CN100433198C (en) | 2008-11-12 |
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