CN102031467B - Method for preparing in-situ deformation Cu-Ag composite material by using magnetic field - Google Patents
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Abstract
The invention relates to a method for preparing an in-situ deformation Cu-Ag composite material by using a magnetic field, belonging to the technical field of materials and comprising the following steps of: 1, with oxygen-free copper and electrolyzed silver as raw materials, preparing a Cu-Ag alloy liquid or Cu-Ag alloy ingot; 2, placing the Cu-Ag alloy liquid or Cu-Ag alloy ingot into a vacuum electric furnace, preserving the temperature and then cooling with the furnace, applying a static magnetic field or alternating-current magnetic field to obtain an as-cast Cu-Ag alloy; 3, preserving the temperature of the as-cast Cu-Ag alloy and then thermally forging to prepare a deformation Cu-Ag alloy; 4, drawing the formation Cu-Ag alloy to prepare a deformation Cu-Ag composite material; 5, thermally treating the deformation Cu-Ag composite material in vacuum, then drawing again; and 6, sequentially repeating the step 5 to obtain the in-situ deformation Cu-Ag composite material. The method provided by the invention effectively improves the ultimate tensile strength and the electric conductivity of the Cu-Ag alloy; and the prepared composite material has greatly improved property.
Description
Technical field
The invention belongs to the material technology field, particularly a kind of method of utilizing magnetic field to prepare original position deformation Cu-Ag matrix material.
Background technology
High-strength high-conductivity Cu based composites is mainly used in bullet train osculatory, circuit lead frame material, high impulse magnet coil and electrical contact material field, is that a kind of intensity and electric conductivity combine structure function material preferably.Yet this type of material is in the course of processing, and the increase electric conductivity with intensity can significantly descend usually, and how in strongthener intensity, to keep higher electric conductivity is the key of this type of investigation of materials.Existing research mainly is chosen in the Cu matrix adds the less transition element of solid solubility, like fcc metallic elements such as bcc metal such as Nb, Cr, Fe and Ag.Yet the Cu-Ag alloy has the following advantages than Cu-bcc class alloy: (1) is in deformation process; Increase with deformation quantity; Cu, Ag two have identical crystalline structure mutually, compatible deformation takes place, so the work hardening rate of Cu-Ag matrix material are faster than matrix materials such as Cu-Nb; (2) the Cu-Ag alloy melting point is low, melting easily, and microtexture is controlled easily; (3) electroconductibility of Ag is better.Therefore the Cu-Ag alloy is wherein more excellent candidate material.In addition; Research shows that the tensile strength of original position deformation Cu-Ag matrix material is relevant with content with the interior nanometer Ag precipitated phase size of electric conductivity and Cu matrix; Precipitated phase is more, tiny more; Fiber strengthening effect after the drawing is good more, and solute atoms separate out the solid solution scattering that also helps reducing electronics, improve specific conductivity.
At present, the more domestic report that have been arranged about preparation deformation in-situ Cu-Ag matrix material.China's application number is that the patent of invention of ZL200510048639.8 discloses a kind of original position deformation Cu-Ag-RE alloy and technology of preparing; Utilize trace rare-earth element the interpolation refinement as-cast structure of alloy; Make the strength of materials reach 1500MPa through repeatedly intermediate heat treatment and gross distortion processing; Electric conductivity reaches 60%IACS, and this patent mainly is to utilize REE refined cast structure, thereby in follow-up drawing, improves the intensity of material.China's application number number discloses the solid solution aging treatment process that the cold drawing of Cu-(7-12) %Ag alloy is processed for the patent of invention of ZL200810060775.2; Cooperate technology to make the intensity of material reach 380 ~ 1400MPa through the solid solution aging processing with cold drawing; Electric conductivity is 60 ~ 92%IACS, and this technology is to utilize solid solution aging to handle to combine the cold drawing technology to improve the intensity and the electric conductivity of material.In recent years; Continuous development along with electromagnetic field technology; Magnetic field technique is being applied aspect the control of material solidification microtexture, and steady magnetic field or induction stirring can be controlled the convection current in the melt, thinning solidification structure; Can also control the solute diffusion and reduce component segregation, and not relate to the preparation of Cu-Ag matrix material under steady magnetic field or the function composite by electromagnetic stirring in the existing document.
Summary of the invention
To the present situation of prior art, the present invention provides the preparation method of original position deformation Cu-Ag matrix material under a kind of the action of a magnetic field, prepares the good Cu-Ag structure function material of intensity and electric conductivity coupling.
Method of the present invention is carried out according to the following steps:
1, be raw material with oxygen free copper and electrolytic silver, process Cu-Ag alloy liquid after the melting, or melting is after the Cu-Ag alloy pig is processed in cooling; The composition of Cu-Ag alloy liquid or Cu-Ag alloy pig is Ag 6 ~ 25% by weight percentage, and surplus is Cu;
2, Cu-Ag alloy pig or Cu-Ag alloy liquid are placed vacuum electric furnace, Cu-Ag alloy pig or Cu-Ag alloy liquid are heated to 960 ~ 1200 ℃, be incubated 0.05 ~ 1 hour, furnace cooling obtains as cast condition Cu-Ag alloy then; In insulation and furnace cooling process, it is that 0.01 ~ 0.2T, frequency are the AC magnetic field of 1 ~ 50Hz that vacuum electric furnace is applied steady magnetic field or the maximum strength that intensity is 1 ~ 20T;
3, as cast condition Cu-Ag alloy is incubated 0.5 ~ 1 hour under 700 ~ 850 ℃ of conditions, then 650 ~ 850 ℃ of forge hots, processes deformation Cu-Ag alloy, the draft of control deformation Cu-Ag alloy is 5 ~ 10%;
4, deformation Cu-Ag alloy is carried out drawing at ambient temperature, keep the drawing direction vertical with the forge hot direction, process deformation Cu-Ag matrix material, total draft of control deformation Cu-Ag matrix material is 65 ~ 85%;
5, deformation Cu-Ag matrix material is carried out vacuum heat treatment, requiring thermal treatment temp is 350 ~ 550 ℃, and heat treatment time is 0.5 ~ 2 hour, and vacuum condition is 10
-5~ 10
-2Pa; Cu-Ag matrix material to after the thermal treatment carries out room temperature drawing once more, and the drawing direction is identical with the drawing direction of step 4, and the total draft of control deformation Cu-Ag matrix material is 80 ~ 98%;
6, repeating step 5 successively, to the cross-sectional diameter of Cu-Ag matrix material be 0.2 ~ 3.0mm, obtain original position deformation Cu-Ag matrix material.
The original position deformation Cu-Ag composite material tensile strength of the present invention's preparation is 550 ~ 1560MPa, and electric conductivity is 65 ~ 95%IACS.
The equipment that melting is adopted in the aforesaid method is vacuum induction melting furnace.
Vacuum electric furnace is meant vacuum resistance furnace or induction furnace in the aforesaid method.
The equipment that applies direct magnetic field in the aforesaid method is superconducting magnet or water-cooled magnet, and the equipment that applies AC magnetic field is magnetic stirrer.
The invention has the beneficial effects as follows: (1) applies magnetic field in the process of setting of Cu-Ag binary alloy, through magnetic field control melt convection, can reach refinement Cu dendrite purpose; (2), can reach and reduce the Ag atom in the intravital solid solution of Cu base through the convection current diffusion of direct magnetic field inhibition solute; (3) quicken the Ag atom through the high-intensity magnetic field energy of magnetization and from Cu, separate out, reduce the solid solubility of Ag in matrix, increase actual effect and strengthen, reduce the solid solution scattering of conduction electrons.
Description of drawings
The as cast condition Cu-Ag alloy macrograph figure that Fig. 1 obtains when adopting no the action of a magnetic field;
Fig. 2 is the as cast condition Cu-Ag alloy macrograph figure that obtains in the embodiment of the invention 3;
Fig. 3 does not handle the as cast condition Cu-Ag alloy macrograph figure that obtains for not carrying out induction stirring;
Fig. 4 is the as cast condition Cu-Ag alloy macrograph figure in the embodiment of the invention 6.
Embodiment
The vacuum induction melting furnace model that adopts in the embodiment of the invention is TG100A-25.
The equipment that applies steady magnetic field in the embodiment of the invention 1,3 is the JMTD-12T100 superconducting magnet.
The equipment that applies steady magnetic field in the embodiment of the invention 2 is the JSD-20T52 superconducting magnet.
The equipment that thermal treatment is adopted in the embodiment of the invention is VHT-II type vacuum heat treatment furnace.
The magnetic stirrer model that adopts in the embodiment of the invention is DJ I/S T-1525Z.
Oxygen free copper that adopts in the embodiment of the invention and electrolytic silver are commercial product, and oxygen free copper weight purity is more than 99.97%, and electrolytic silver weight purity is more than 99.996%.
As cast condition Cu-Ag alloy is the right cylinder of diameter 10 ~ 30mm in the embodiment of the invention, and forge hot is carried out along the axial vertical direction of as cast condition Cu-Ag alloy, and cold-drawn is axially carried out along as cast condition Cu-Ag alloy.
Embodiment 1
With oxygen free copper and electrolytic silver is raw material, processes Cu-Ag alloy liquid after the melting, and the composition of Cu-Ag alloy liquid is Ag 6% by weight percentage, and surplus is Cu;
Cu-Ag alloy liquid is placed vacuum resistance furnace, Cu-Ag alloy liquid is heated to 1200 ℃, be incubated 1 hour, furnace cooling obtains as cast condition Cu-Ag alloy then; In insulation and furnace cooling process, vacuum resistance furnace is applied the steady magnetic field that magnetic induction density is 1T;
850 ℃ of insulations 0.5 hour, deformation Cu-Ag alloy was processed in forge hot under 650 ~ 850 ℃ of conditions then with as cast condition Cu-Ag alloy, and the control draft is 10%;
Deformation Cu-Ag alloy is carried out drawing at ambient temperature, keep the drawing direction vertical with the forge hot direction, process deformation Cu-Ag matrix material, controlling total draft is 65%;
Deformation Cu-Ag matrix material is carried out vacuum heat treatment, and requiring thermal treatment temp is 350 ℃, and heat treatment time is 0.5 hour, and vacuum condition is 10
-2Pa;
Cu-Ag matrix material to after the thermal treatment carries out room temperature drawing once more, and the drawing direction is identical with last time drawing direction, and the total draft of control deformation Cu-Ag matrix material is 80%;
Repeating vacuum thermal treatment and room temperature drawing step once more, to the cross-sectional diameter of Cu-Ag matrix material be 3.0mm, obtain original position deformation Cu-Ag matrix material; Its tensile strength is 550MPa, and electric conductivity is 95%IACS.
Embodiment 2
With oxygen free copper and electrolytic silver is raw material, and melting is after the Cu-Ag alloy pig is processed in cooling; The composition of Cu-Ag alloy pig is Ag 14% by weight percentage, and surplus is Cu;
The Cu-Ag alloy pig is placed vacuum resistance furnace, the Cu-Ag alloy pig is heated to 980 ℃, be incubated 0.3 hour, furnace cooling obtains as cast condition Cu-Ag alloy then; In insulation and furnace cooling process, vacuum resistance furnace is applied the steady magnetic field that magnetic induction density is 20T;
As cast condition Cu-Ag alloy is incubated 0.8 hour under 800 ℃ of conditions, deformation Cu-Ag alloy is processed in forge hot under 650 ~ 850 ℃ of conditions then, and the control draft is 9%;
Deformation Cu-Ag alloy is carried out drawing at ambient temperature, keep the drawing direction vertical with the forge hot direction, process deformation Cu-Ag matrix material, total draft of control deformation Cu-Ag matrix material is 70%;
Deformation Cu-Ag matrix material is carried out vacuum heat treatment, and requiring thermal treatment temp is 400 ℃, and heat treatment time is 1 hour, and vacuum condition is 3 * 10
-3Pa;
Cu-Ag matrix material to after the thermal treatment carries out room temperature drawing once more, and the drawing direction is identical with last time drawing direction, and the total draft of control deformation Cu-Ag matrix material is 90%;
Repeating vacuum thermal treatment and room temperature drawing step once more, to the cross-sectional diameter of Cu-Ag matrix material be 1.0mm, obtain original position deformation Cu-Ag matrix material; Its tensile strength is 950MPa, and electric conductivity is 80%IACS.
Embodiment 3
With oxygen free copper and electrolytic silver is raw material, processes Cu-Ag alloy liquid after the melting, and the composition of Cu-Ag alloy liquid is Ag25% by weight percentage, and surplus is Cu;
Cu-Ag alloy liquid is placed vacuum resistance furnace, Cu-Ag alloy liquid is heated to 960 ℃, be incubated 0.05 hour, furnace cooling obtains as cast condition Cu-Ag alloy then; In insulation and furnace cooling process, vacuum resistance furnace is applied the steady magnetic field that magnetic induction density is 12T; As cast condition Cu-Ag alloy macrograph is as shown in Figure 2;
As cast condition Cu-Ag alloy is incubated 1 hour under 750 ℃ of conditions, deformation Cu-Ag alloy is processed in forge hot under 650 ~ 850 ℃ of conditions then, and the draft of control deformation Cu-Ag alloy is 5%;
Deformation Cu-Ag alloy is carried out drawing at ambient temperature, keep the drawing direction vertical with the forge hot direction, process deformation Cu-Ag matrix material, total draft of control deformation Cu-Ag matrix material is 85%;
Deformation Cu-Ag matrix material is carried out vacuum heat treatment, and requiring thermal treatment temp is 350 ~ 550 ℃, and heat treatment time is 0.5 ~ 2 hour, and vacuum condition is 10
-5Pa;
Cu-Ag matrix material to after the thermal treatment carries out room temperature drawing once more, and the drawing direction is identical with last time drawing direction, and the total draft of control deformation Cu-Ag matrix material is 98%;
Repeating vacuum thermal treatment and room temperature drawing step once more, to the cross-sectional diameter of Cu-Ag matrix material be 0.2mm, obtain original position deformation Cu-Ag matrix material; Its tensile strength is 1510MPa, and electric conductivity is 65%IACS;
Adopt homogeneous raw material to prepare Cu-Ag alloy liquid, prepare as cast condition Cu-Ag alloy then in a manner described, difference is not apply steady magnetic field, and the as cast condition Cu-Ag alloy macrograph of acquisition is as shown in Figure 2.
Embodiment 4
With oxygen free copper and electrolytic silver is raw material, and melting is after the Cu-Ag alloy pig is processed in cooling; The composition of Cu-Ag alloy pig is Ag 6% by weight percentage, and surplus is Cu;
The Cu-Ag alloy pig is placed induction furnace, the Cu-Ag alloy pig is heated to 960 ℃, be incubated 1 hour, furnace cooling obtains as cast condition Cu-Ag alloy then; In insulation and furnace cooling process, adopting magnetic stirrer that induction furnace is applied maximum magnetic induction is that 0.01T, frequency are the AC magnetic field of 2Hz;
As cast condition Cu-Ag alloy is incubated 0.8 hour under 750 ℃ of conditions, deformation Cu-Ag alloy is processed in forge hot under 650 ~ 850 ℃ of conditions then, and the control draft is 10%;
Deformation Cu-Ag alloy is carried out drawing at ambient temperature, keep the drawing direction vertical with the forge hot direction, process deformation Cu-Ag matrix material, controlling total draft is 65%;
Deformation Cu-Ag matrix material is carried out vacuum heat treatment, and requiring thermal treatment temp is 450 ℃, and heat treatment time is 1.5 hours, and vacuum condition is 10
-5Pa;
Cu-Ag matrix material to after the thermal treatment carries out room temperature drawing once more, and the drawing direction is identical with last time drawing direction, and to control total draft be 80%;
Repeating vacuum thermal treatment and room temperature drawing step once more, to the cross-sectional diameter of Cu-Ag matrix material be 3.0mm, obtain original position deformation Cu-Ag matrix material; Its tensile strength is 915MPa, and electric conductivity is 85%IACS.
With oxygen free copper and electrolytic silver is raw material, processes Cu-Ag alloy liquid after the melting, and Cu-Ag alloy liquid composition is Ag 14% by weight percentage, and surplus is Cu;
Cu-Ag alloy liquid is placed vacuum resistance furnace, and general or Cu-Ag alloy liquid are heated to 1100 ℃, are incubated 0.2 hour, and furnace cooling obtains as cast condition Cu-Ag alloy then; In insulation and furnace cooling process, adopting magnetic stirrer that induction furnace is applied maximum magnetic induction is that 0.2T, frequency are the AC magnetic field of 32Hz;
As cast condition Cu-Ag alloy is incubated 0.5 hour under 800 ℃ of conditions, deformation Cu-Ag alloy is processed in forge hot under 650 ~ 850 ℃ of conditions then, and the control draft is 8%;
Deformation Cu-Ag alloy is carried out drawing at ambient temperature, keep the drawing direction vertical with the forge hot direction, process deformation Cu-Ag matrix material, controlling total draft is 80%;
Deformation Cu-Ag matrix material is carried out vacuum heat treatment, and requiring thermal treatment temp is 350 ℃, and heat treatment time is 2 hours, and vacuum condition is 10
-3Pa;
Cu-Ag matrix material to after the thermal treatment carries out room temperature drawing once more, and the drawing direction is identical with last time drawing direction, and to control total draft be 95%;
Repeating vacuum thermal treatment and room temperature drawing step once more, to the cross-sectional diameter of Cu-Ag matrix material be 0.2mm, obtain original position deformation Cu-Ag matrix material; Its tensile strength is 1150MPa, and electric conductivity is 78%IACS.
Embodiment 6
With oxygen free copper and electrolytic silver is raw material, and melting is after the Cu-Ag alloy pig is processed in cooling; The composition of Cu-Ag alloy pig is Ag25% by weight percentage, and surplus is Cu;
The Cu-Ag alloy pig is placed vacuum resistance furnace, the Cu-Ag alloy pig is heated to 1200 ℃, be incubated 0.05 hour, furnace cooling obtains as cast condition Cu-Ag alloy then; In insulation and furnace cooling process, adopting magnetic stirrer that induction furnace is applied maximum magnetic induction is that 0.1T, frequency are the AC magnetic field of 8Hz.As cast condition Cu-Ag alloy macrograph is as shown in Figure 4;
As cast condition Cu-Ag alloy is incubated 1 hour under 700 ℃ of conditions, deformation Cu-Ag alloy is processed in forge hot under 650 ~ 850 ℃ of conditions then, and the draft of control deformation Cu-Ag alloy is 5%;
Deformation Cu-Ag alloy is carried out drawing at ambient temperature, keep the drawing direction vertical with the forge hot direction, process deformation Cu-Ag matrix material, controlling total draft is 85%;
Deformation Cu-Ag matrix material is carried out vacuum heat treatment, and requiring thermal treatment temp is 550 ℃, and heat treatment time is 0.5 hour, and vacuum condition is 10
-2Pa;
Cu-Ag matrix material to after the thermal treatment carries out room temperature drawing once more, and the drawing direction is identical with last time drawing direction, and to control total draft be 98%;
Repeating vacuum thermal treatment and room temperature drawing step once more, to the cross-sectional diameter of Cu-Ag matrix material be 0.5mm, obtain original position deformation Cu-Ag matrix material; Its tensile strength is 1380MPa, and electric conductivity is 76%IACS;
Adopt homogeneous raw material to prepare the Cu-Ag alloy pig, prepare as cast condition Cu-Ag alloy then in a manner described, difference is not apply AC magnetic field, and the as cast condition Cu-Ag alloy macrograph of acquisition is as shown in Figure 3.The solid solution scattering of electricity electronics.
Claims (2)
1. method of utilizing magnetic field to prepare original position deformation Cu-Ag matrix material is characterized in that carrying out according to the following steps:
(1) be raw material with oxygen free copper and electrolytic silver, process Cu-Ag alloy liquid after the melting, or melting is after the Cu-Ag alloy pig is processed in cooling; The composition of Cu-Ag alloy liquid or Cu-Ag alloy pig is Ag 6 ~ 25% by weight percentage, and surplus is Cu;
(2) Cu-Ag alloy pig or Cu-Ag alloy liquid are placed vacuum electric furnace, Cu-Ag alloy pig or Cu-Ag alloy liquid are heated to 960 ~ 1200 ℃, be incubated 0.05 ~ 1 hour, furnace cooling obtains as cast condition Cu-Ag alloy then; In insulation and furnace cooling process, vacuum electric furnace being applied steady magnetic field or the maximum strength that intensity is 1 ~ 20T is that 0.01 ~ 0.2T, frequency are the AC magnetic field of 1 ~ 50Hz;
(3) as cast condition Cu-Ag alloy is incubated 0.5 ~ 1 hour under 700 ~ 850 ℃ of conditions, then 650 ~ 850 ℃ of forge hots, processes deformation Cu-Ag alloy, the draft of control deformation Cu-Ag alloy is 5 ~ 10%;
(4) deformation Cu-Ag alloy is carried out drawing at ambient temperature, keep the drawing direction vertical with the forge hot direction, process deformation Cu-Ag matrix material, total draft of control deformation Cu-Ag matrix material is 65 ~ 85%;
(5) deformation Cu-Ag matrix material is carried out vacuum heat treatment, requiring thermal treatment temp is 350 ~ 550 ℃, and heat treatment time is 0.5 ~ 2 hour, and vacuum condition is 10
-5~ 10
-2Pa; Cu-Ag matrix material to after the thermal treatment carries out room temperature drawing once more, and the drawing direction is identical with the drawing direction of step (4), and the total draft of control deformation Cu-Ag matrix material is 80 ~ 98%;
(6) repeating step (5) successively, to the cross-sectional diameter of Cu-Ag matrix material be 0.2 ~ 3.0mm, obtain original position deformation Cu-Ag matrix material.
2. a kind of method of utilizing magnetic field to prepare original position deformation Cu-Ag matrix material according to claim 1 is characterized in that described original position deformation Cu-Ag composite material tensile strength is 550 ~ 1560MPa, and electric conductivity is 65 ~ 95%IACS.
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| CN102400007B (en) * | 2011-11-29 | 2014-05-14 | 东北大学 | Eutectic strengthening reinforced Cu-Ag alloy and preparation method thereof |
| CN105839038B (en) * | 2016-04-08 | 2017-06-30 | 东北大学 | A kind of preparation method of high-strength high-conductivity Cu Ag Fe alloys |
| CN106676314B (en) * | 2016-12-28 | 2018-06-15 | 北京有色金属研究总院 | A kind of preparation method of high-strength high-conductivity Cu-Ag alloys |
| JPWO2019013163A1 (en) * | 2017-07-10 | 2020-02-06 | 株式会社協成 | Conductive member, contact pin and device using copper-silver alloy |
| CN108823464B (en) * | 2018-07-02 | 2020-10-09 | 上海电缆研究所有限公司 | Copper alloy material and preparation method thereof |
| CN114318048A (en) * | 2021-12-16 | 2022-04-12 | 镇江市镇特合金材料有限公司 | Copper alloy for conductive tile with high welding performance and preparation method thereof |
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