CN101104896A - Fibre composite reinforcement Cu-Fe-RE alloy and preparation method thereof - Google Patents
Fibre composite reinforcement Cu-Fe-RE alloy and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a fiber composite-reinforced Cu-Fe-RE alloy and the preparation method thereof. The chemical components of the material comprise 3-10 percent of Fe, 0.03-0.3 percent of mixed rare earth and Cu in balance. The preparation method comprises melting Cu and Fe in a vacuum induction furnace below a residual gas pressure of 0.1Pa, introducing Ar until the pressure reaches 30-50KPa, adding mixed rare earth to allow molten, casting to obtain ingot, performing multi-pass room-temperature drawing while controlling the degree of drawing deformation (carrying out the intermediate heat treatment for three times during the drawing process), and stopping when the deformation degree Eta is equal to 8.0 to obtain an alloy with diphase fiber composite-reinforced structure. With this method, the nanofiber composite-reinforced alloy is free of noble alloy elements and has features of efficient refining of the original structure in the rare earth microalloying method. The method can keep the mechanical property and electrical conductivity of the material at higher level while reducing the material cost and simplifying the production process.
Description
Technical field
The present invention relates to a kind of copper base alloy and technology of preparing thereof.Especially relate to a kind of nanofiber complex intensifying Cu-Fe alloy and technology of preparing thereof that contains rare earth element.
Background technology
Progress of science and technology is more and more higher to the electro-conductive material performance demands.For example, the conductor coils that high-tech area medium-high magnetic field technology is used and the lead frame of large-scale integrated circuit still have good electrical conductivity when requirement can be born very high loads.The working conditions of the not competent this harshness of conventional conductor material, the conductor material that necessarily requires high strength more to have excellent conductive performance simultaneously concurrently satisfies the development need of this type of science and technology field.
The intensity of conductor material and electroconductibility generally are the inverse function relation, and promptly improving intensity is cost with heavy losses electroconductibility often.Therefore, making great efforts to make material to keep high conductivity or can improve intensity significantly but only sacrifice electroconductibility on a small quantity, is the focus of developing the novel conductor material at present.By in the Cu matrix, adding immiscible alloying element, and the fiber phase complex intensifying copper alloy by the preparation of strong strain process, be considered to the most rising high-strength highly-conductive material at present, having developed than conventional material at present has the more conductor wires of premium properties.In this class material, alloys such as Cu-Ag and Cu-Nb have preferable intensity and electroconductibility matching relationship, thereby are subjected to enough attention at home and abroad.Yet these materials consumption precious metal resources are more, increased considerably material cost, use to be subjected to bigger restriction.Comparatively speaking, the Cu-Fe cost of alloy is lower, have a extensive future, but intensity and conductivity coupling level is limited, and the strain fibrosis course of processing is difficulty relatively, need further improve.Rare earth element has favourable alloying effect in the Cu alloy, can improve alloy organizing and performance by adding rare earth element.
Patent ZL02110785.8 has invented a kind of fibre heterogeneous reinforced rare earth Cu-Ag alloy, by in alloy, adding (0.14～0.20) % (mass percent, rare earth element down together), after drawing deformation and intermediate heat treatment, form fiber composite tissue, make alloy under the situation that contains the minimizing of Ag amount, still can reach and contain the higher alloy property level of Ag amount.Patent (application number: 200510026596.3) announced a kind of preparation method of composite Cu-Fe-Ag nano material at original position with high intensity and high conductance, the reasonable distribution that adopt that sonic oscillation solidifies, preparation methods such as deformation processing, solid solution and interrupted aging causes nanofiber and precipitation particles strengthening phase in the alloy structure is to guarantee alloy property.Though these two kinds of alloys all have fiber composite tissue and good performance level, but still contain the Ag up to about 6%, and also more complicated of the course of processing.
Patent ZL03114720.8 has invented a kind of Cu base high-strength highly-conductive material and preparation technology thereof, added (0.02～2.0) %Fe in the alloy, (0.01～0.1) %P, (0.001～0.1) %B and (0.001～1.0) % rare earth or lucium, the purification of comprehensive utilization metal melt, refined crystalline strengthening, precipitation strength and dislocations strengthening effect obtain superperformance.U.S. Pat 6506269 has been invented a kind of high-strength highly-conductive Cu-(Ni, Co, Fe)-the Si Alloy And Preparation Method, contain (0.5～2.5) %Ni in the alloy, (0.5～2.5) %Co, (0.5～0.8) %Si and (0.05～0.15) % (Mg+p) by timeliness with cold rollingly can reach specific conductivity that is higher than 65%IACS and the tensile strength that is higher than 600MPa, are exclusively used in lead frame.U.S. Pat 5215711 has been invented a kind of age hardening type Cu-(0.01～10) %Fe alloy, wherein contains (1～2.5) %Ni in addition, (0.01～7) %Si, (0.01～7) %Ti and (0.001～1) %B.Yet these alloys mainly rely on forging and roll forming and can not form the tissue with the compound characteristics of linear nanofiber, and alloy element component and preparation process be more complicated also.
U.S. Pat 5043025 has been invented a kind of high-strength highly-conductive Cu-Fe matrix material, rely on mixing, pre-compacted (hot and cold etc. static pressure or hot extrusion), hydrogen reduction processing and the press working technological processs such as (die forging, rolling or drawings) of Cu and two kinds of powder of about 15%Fe to make the alloy material of fibre composite reinforcement, its characteristics are that the temperature and time that can control recombination process prevents that the Fe solute atoms from dissolving in the Cu matrix, to avoid damaging conductivity.This material require utilizes rare gas element powder process, prevents process procedure more complicated such as powder granule surface oxidation and pollution and particle size control, and industrial production is difficulty relatively, and cost is higher.
Related to fibre composite reinforcement Cu-Fe alloy and technology of preparing thereof in some academic papers of having delivered, with comparatively relevant the having of the present invention: Yamaguchi etc. (Metall.Trans., 1971,2:1293); Verhoeven etc. (J.Mater.Sci., 1989,24:1748); Jerman etc. (Metall.Trans.1993,24A:35); Spitzig etc. (J.Mater.Sci., 1992,27:2005); Biselli etc. (Acta Mater., 1996,44:493); (J.Mater.Proc.Technl., 2001,113:610 such as Song; J.Alloys Comp., 2005,388:69; J.Alloys Comp., 2000,311:265); (Scr.Mater., 2001,45:1295 such as Hong; Metall.Mater.Trans., 2001,32A:985); Ge Ji equality (Dalian Railway University's journal, 2003,24:71; The material heat treatment journal, 2005,26:14); High petrel etc. (the matrix material journal, 2006,23:120).Yet the alloy that these papers are studied does not all comprise the alloying of rare earth element and contains the technology of preparing of rare earth element Cu-Fe fiber composite tissue.
Summary of the invention
At disadvantages of background technology, the object of the present invention is to provide a kind of fibre composite reinforcement Cu-Fe-RE alloy and preparation method thereof, carry out microalloying by the mixed rare-earth elements that the Cu-Fe alloy is added certain content, refinement is initially organized, adopt technologies such as drawing deformation and intermediate heat treatment, obtain having the weave construction of nanometer complex phase fiber strengthening characteristics.
The technical scheme that the present invention solves its technical problem employing is:
One, a kind of fibre composite reinforcement Cu-Fe-RE alloy:
The mass percent of each component is 3%～10%Fe, 0.03%～0.3% mishmetal, and all the other are Cu.
The mass percent of each component is 50%Ce in the described mishmetal, 16%Nd, and 8%Pr, all the other are La.
Two, a kind of preparation method of fibre composite reinforcement Cu-Fe-RE alloy, the step of this method is as follows:
(1) vacuum induction furnace that places residual gas pressure to be lower than 0.1Pa electrolytic copper, technically pure iron melts;
(2) fill Ar after the solution left standstill degasification in stove, add mixed rare-earth elements, fusing and induction stirring be the back casting ingot-forming evenly;
(3) with ingot casting multi-pass drawing at room temperature, in drawing process, adopt three intermediate heat treatment, final deformation extent is η=8.0.
In the described step (2), filling Ar pressure in adding the mixed rare-earth elements forehearth is 30～50kPa.
In the drawing deformation process of described step (3), when deformation extent η＜3.0, drawing passes average deformation degree η＜0.10～0.15; When deformation extent η 〉=3.0, drawing passes average deformation degree η＜0.08～0.11.
Three intermediate heat treatment technologies of described step (3) are: when η=1.0 at 440 ℃ of annealing 2 h, when η=2.0 at 380 ℃ of annealing 4h, when η=3.0 at 360 ℃ of annealing 4h.
The beneficial effect that the present invention has:
(1) do not contain expensive alloy element, alloying constituent is simple relatively, can reduce material cost, is beneficial to production;
(2) only need drawing and intermediate heat treatment process can form the nanofiber complex tissue, need not links such as powder process, hot isostatic pressing and hot-work predeformation, machining process is simplified relatively;
(3) with the microalloying of rare earth method effectively refinement original structure, under the condition that reduces material cost and simplified processing process, make material property still remain on higher level.
Embodiment
Embodiment 1:
With 3% technically pure iron of given mass percent proportioning, 0.03% mishmetal, all the other are the pickling of electrolytic copper starting material and fully clean the back oven dry;
Cu, Fe are placed vacuum induction furnace, after leaving standstill degasification, fusing in stove, fills Ar to 30kPa being lower than under the 0.1Pa normal atmosphere, evenly add mixed rare-earth elements again through induction stirring, leave standstill the column ingot casting that 2～3min pours into diameter of phi 25.0mm after fusing and the induction stirring;
Multi-pass drawing at room temperature after the surface imperfection is removed in turning processing, when deformation extent η＜3.0, and drawing passes average deformation degree η＜0.15; When deformation extent η 〉=3.0, drawing passes average deformation degree η＜0.11;
Carry out intermediate heat treatment in the drawing process 3 times: when η=1.0 at 440 ℃ of annealing 2h; When η=2.0 at 380 ℃ of annealing 4h; When η=3.0 at 360 ℃ of annealing 4h.Final deformation extent is η=8.0.
Embodiment 2:
With 6% technically pure iron of given mass percent proportioning, 0.1% mishmetal, all the other are the pickling of electrolytic copper starting material and fully clean the back oven dry;
Cu, Fe are placed vacuum induction furnace, after leaving standstill degasification, fusing in stove, fills Ar to 40kPa being lower than under the 0.1Pa normal atmosphere, evenly add mixed rare-earth elements again through induction stirring, leave standstill the column ingot casting that 2～3min pours into diameter of phi 25.0mm after fusing and the induction stirring;
Multi-pass drawing at room temperature after the surface imperfection is removed in turning processing, when deformation extent η＜3.0, and drawing passes average deformation degree η＜0.12; When deformation extent η 〉=3.0, drawing passes average deformation degree η＜0.09;
Carry out intermediate heat treatment in the drawing process 3 times: when η=1.0 at 440 ℃ of annealing 2h; When η=2.0 at 380 ℃ of annealing 4h; When η=3.0 at 360 ℃ of annealing 4h.Final deformation extent is η=8.0.
Embodiment 3:
With 10% technically pure iron of given mass percent proportioning, 0.3% mishmetal, all the other are the pickling of electrolytic copper starting material and fully clean the back oven dry;
Cu, Fe are placed vacuum induction furnace, after leaving standstill degasification, fusing in stove, fills Ar to 50kPa being lower than under the 0.1Pa normal atmosphere, evenly add mixed rare-earth elements again through induction stirring, leave standstill the column ingot casting that 2～3min pours into diameter of phi 25.0mm after fusing and the induction stirring;
Multi-pass drawing at room temperature after the surface imperfection is removed in turning processing, when deformation extent η＜3.0, and drawing passes average deformation degree η＜0.10; When deformation extent η 〉=3.0, drawing passes average deformation degree η＜0.08;
Carry out intermediate heat treatment in the drawing process 3 times: when η=1.0 at 440 ℃ of annealing 2h; When η=2.0 at 380 ℃ of annealing 4h; When η=3.0 at 360 ℃ of annealing 4h.Final deformation extent is η=8.0.
The concrete numerical value of three embodiment is as follows shown in the table 1 of face.
The composition of table 1 alloy of the present invention, tissue and examples of properties
| Embodiment | Alloying element (%) | The original structure parameter | Performance perameter | |||||
| Fe | RE | Cu | Average grain size (μ m) | Average dendrite interval (μ m) | Tensile strength (MPa) | Hardness (HV) | Relative conductivity (%IACS) | |
| 1 | 3 | 0.03 | All the other | 22～35 | 12～20 | 650～750 | 120～134 | 55～61 |
| 2 | 6 | 0.1 | All the other | 18～30 | 12～18 | 780～830 | 140～150 | 58～65 |
| 3 | 10 | 0.3 | All the other | 16～25 | 10～17 | 880～950 | 150～165 | 56～62 |
| The simultaneous test alloy that does not contain rare earth | 6 | - | All the other | 35～44 | 18～23 | 720～780 | 130～140 | 50～58 |
As can be seen from Table 1, with the microalloying of rare earth method effectively refinement original structure, under the condition that reduces material cost and simplified processing process, make material property still remain on higher level.
Claims (6)
1. fibre composite reinforcement Cu-Fe-RE alloy, it is characterized in that: the mass percent of each component is 3%～10%Fe, 0.03%～0.3% mishmetal, all the other are Cu.
2. a kind of fibre composite reinforcement Cu-Fe-RE alloy according to claim 1 is characterized in that: the mass percent of each component is 50%Ce in the described mishmetal, 16%Nd, and 8%Pr, all the other are La.
3. the preparation method who is used for the described fibre composite reinforcement Cu-Fe-RE alloy of claim 1 is characterized in that the step of this method is as follows:
(1) vacuum induction furnace that places residual gas pressure to be lower than 0.1Pa electrolytic copper, technically pure iron melts;
(2) fill Ar after the solution left standstill degasification in stove, add mixed rare-earth elements, fusing and induction stirring be the back casting ingot-forming evenly;
(3) with ingot casting multi-pass drawing at room temperature, in drawing process, adopt three intermediate heat treatment, final deformation extent is η=8.0.
4. the preparation method of a kind of fibre composite reinforcement Cu-Fe-RE alloy of fibre according to claim 3 is characterized in that: in the described step (2), filling Ar pressure in adding the mixed rare-earth elements forehearth is 30～50kPa.
5. the preparation method of a kind of fibre composite reinforcement Cu-Fe-RE alloy of fibre according to claim 3 is characterized in that: in the drawing deformation process of described step (3), and when deformation extent η＜3.0, drawing passes average deformation degree η＜0.10～0.15; When deformation extent η 〉=3.0, drawing passes average deformation degree η＜0.08～0.11.
6. fibre composite reinforcement Cu-Fe-RE alloy according to claim 3 and technology of preparing thereof, it is characterized in that: three intermediate heat treatment technologies of described step (3) are: when η=1.0 at 440 ℃ of annealing 2h, when η=2.0 at 380 ℃ of annealing 4h, when η=3.0 at 360 ℃ of annealing 4h.
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| CN109852822A (en) * | 2019-01-29 | 2019-06-07 | 常州和昶特种合金有限公司 | A method of preparing copper and iron composite functional material |
| CN111826545A (en) * | 2020-06-24 | 2020-10-27 | 东南大学 | Copper-iron alloy material and preparation method and application thereof |
| CN111549253A (en) * | 2020-07-03 | 2020-08-18 | 江西省科学院应用物理研究所 | Rare earth copper-iron alloy, preparation method and application |
| CN111549253B (en) * | 2020-07-03 | 2021-06-18 | 江西省科学院应用物理研究所 | Rare earth copper-iron alloy, preparation method and application |
| CN113913643A (en) * | 2021-10-13 | 2022-01-11 | 江西金叶大铜科技有限公司 | Cu-Fe-Re in-situ composite reinforced copper alloy material and preparation method thereof |
| CN116694953A (en) * | 2023-08-04 | 2023-09-05 | 中铝科学技术研究院有限公司 | Copper alloy plate strip for electromagnetic shielding and preparation method thereof |
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