CN110284024B - Preparation method of tellurium-copper alloy material - Google Patents

Preparation method of tellurium-copper alloy material Download PDF

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CN110284024B
CN110284024B CN201910716766.2A CN201910716766A CN110284024B CN 110284024 B CN110284024 B CN 110284024B CN 201910716766 A CN201910716766 A CN 201910716766A CN 110284024 B CN110284024 B CN 110284024B
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tellurium
copper alloy
alloy material
copper
extrusion
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CN110284024A (en
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侯龙超
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Chengdu Yunxin Nonferrous Metals Co ltd
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Chengdu Yunxin Nonferrous Metals Co ltd
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B21MECHANICAL METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL; PUNCHING METAL
    • B21CMANUFACTURE OF METAL SHEETS, WIRE, RODS, TUBES OR PROFILES, OTHERWISE THAN BY ROLLING; AUXILIARY OPERATIONS USED IN CONNECTION WITH METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL
    • B21C1/00Manufacture of metal sheets, metal wire, metal rods, metal tubes by drawing
    • B21C1/003Drawing materials of special alloys so far as the composition of the alloy requires or permits special drawing methods or sequences
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C1/00Making non-ferrous alloys
    • C22C1/02Making non-ferrous alloys by melting
    • C22C1/03Making non-ferrous alloys by melting using master alloys
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C9/00Alloys based on copper
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01BCABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
    • H01B1/00Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors
    • H01B1/02Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors mainly consisting of metals or alloys
    • H01B1/026Alloys based on copper
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01BCABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
    • H01B13/00Apparatus or processes specially adapted for manufacturing conductors or cables

Abstract

The invention provides a preparation method of a tellurium-copper alloy material, which comprises the following steps: (1) smelting: adding cathode copper into a smelting furnace, and heating and melting; adding phosphorus copper intermediate alloy for deoxidation after complete melting, then adding tellurium copper intermediate alloy, controlling the furnace temperature at 1250-1260 ℃, adding rare earth elements after heat preservation and standing, adjusting the furnace temperature to 1200-1240 ℃ after complete melting, and casting into ingots through water cooling; (2) carrying out extrusion deformation processing; (3) acid washing and hydraulic drawing; (4) polishing and sizing to obtain the product; the tellurium-copper alloy material comprises the following elements in percentage by weight: 0.15-0.5% of Te; r is 0.08-0.12%; 0.002-0.005% of P; the balance of Cu; r is at least one of rare earth elements of scandium or yttrium. The method can improve the conductivity of the tellurium-copper alloy material and ensure that the tellurium-copper alloy material has higher mechanical strength.

Description

Preparation method of tellurium-copper alloy material
Technical Field
The invention belongs to the technical field of alloy material preparation, and particularly relates to a preparation method of a tellurium-copper alloy material.
Background
Tellurium copper C14500, a high-conductivity free-cutting copper alloy material, has good free-cutting performance, electric conductivity, heat conductivity, corrosion resistance, electric ablation resistance and good cold and hot processing performance. After the second world war, free-cutting copper alloys began to appear with the widespread use of tellurium, and free-cutting alloy materials represented by C14500 copper alloy have excellently solved the problem of difficult processing of high-conductivity copper materials. However, the electrical conductivity of C14500 is only 85-90% ICAS, so when the electrical connector is used for high-voltage and high-current electronic and electrical connector, the temperature of the connector is easily increased and the resistance is increased under a long-time high-load working condition, and finally the electrical contact is failed, so that the service life of the electrical connector is influenced; on the other hand, if the conductivity of the alloy is enhanced, the mechanical property of the alloy material is poor, and the use requirements of other fields are difficult to meet.
Researchers at home and abroad research high-strength and high-conductivity copper alloy materials, and the strengthening method mainly comprises an alloying method and a composite material method: the mechanical property of the copper alloy prepared by the alloying method is improved in a mode of sacrificing the conductivity to a certain extent, and the result of considering both the conductivity and the conductivity cannot be really achieved; the composite material method has the disadvantages of complex processing technology and high production cost, and is still in the experimental research stage at present.
Therefore, it is an urgent technical problem to provide a method for preparing a tellurium-copper alloy material, so as to improve the conductivity of the tellurium-copper alloy material, and simultaneously ensure the mechanical strength of the alloy material, and expand the application of the tellurium-copper alloy material.
Disclosure of Invention
The invention aims to solve the technical problems, and provides a preparation method of a tellurium-copper alloy material, so as to provide a preparation method which can improve the conductivity of the tellurium-copper alloy material and ensure that the tellurium-copper alloy material has higher mechanical strength.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows:
a preparation method of a tellurium-copper alloy material comprises the following steps:
(1) smelting: adding the rest cathode copper with the purity of more than 99.99 percent into a smelting furnace according to the corresponding weight percentage, and heating and melting under the covering protection of a covering agent; after cathode copper is completely melted, adding phosphorus-copper intermediate alloy for deoxidation according to the phosphorus ratio, controlling the furnace temperature to 1150-1170 ℃, keeping the temperature and standing, adding tellurium-copper intermediate alloy, controlling the furnace temperature to 1250-1260 ℃, keeping the temperature and standing, adding rare earth elements, stirring a molten pool after complete melting, adjusting the furnace temperature to 1200-1240 ℃, baking the furnace end for multiple times, and then casting into ingots by water cooling;
(2) extruding: putting the copper alloy ingot obtained in the step (1) into an induction furnace, heating to 830-840 ℃, preserving heat for 30-45 min to uniformly refine crystal grains, and then performing extrusion deformation processing;
(3) acid washing and hydraulic drawing: performing acid washing on the product obtained in the step (2), washing off surface oxides, and then performing hydraulic drawing;
(4) polishing and sizing the section bar after the drawing deformation to obtain the finished product;
the tellurium-copper alloy material comprises the following elements in percentage by weight:
Te 0.15~0.5%;
R 0.08~0.12%;
P 0.002~0.005%;
the balance of Cu;
r is at least one of rare earth elements of scandium or yttrium.
According to the invention, rare earth element scandium or yttrium is introduced into the tellurium-copper alloy, and a preparation process suitable for the alloy material is designed, so that the industrial production application can be well met, and the conductivity and the mechanical property of the obtained alloy material are greatly improved.
Further, in the step (1), the covering agent is one of charcoal, graphite flake or graphite powder.
Further, the phosphor-copper master alloy is CuP 14.
Further, the tellurium copper intermediate alloy is CuTe.
Further, the extrusion deformation processing is carried out on an 800 horizontal extruder, and the specification of the extrusion deformation processing is 1200+15 KW.
Further, the extrusion is carried out in a backward extrusion mode, and the extrusion temperature is 780 +/-10 ℃.
Further, the acid cleaning is to place the billet obtained after extrusion in a sulfuric acid tank with the concentration of 15-20% for acid cleaning.
Further, the hydraulic drawing is carried out in a hydraulic drawing machine, and the specification of the hydraulic drawing machine is 60+18 KW.
Further, the specification of the drawing die for hydraulic drawing is phi 2.5mm and 39 mm.
Due to the adoption of the preparation method, the following beneficial effects are realized:
(1) the conductivity of the tellurium-copper alloy material obtained by the method is up to more than 97 percent;
(2) the mechanical properties of the tellurium-copper alloy material obtained by the method are as follows: the tensile strength Rm is more than or equal to 380MPa, the cutting performance is more than or equal to 90 percent, and the elongation is more than or equal to 22 percent.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more clearly understood, the present invention is described in detail below with reference to the following embodiments, and it should be noted that the following embodiments are only for explaining and illustrating the present invention and are not intended to limit the present invention. The invention is not limited to the embodiments described above, but rather, may be modified within the scope of the invention.
Example 1
The tellurium-copper alloy material comprises the following elements in percentage by weight:
0.15 percent of Te; 0.08 percent of R; 0.002% of P; the balance of Cu; wherein R is rare earth element scandium.
The preparation method of the tellurium-copper alloy material comprises the following steps:
(1) smelting: adding the cathode copper with the purity of 99.99 percent into a smelting furnace according to the corresponding weight percentage, and heating and melting under the protection of covering agent (charcoal); after cathode copper is completely melted, adding a phosphorus-copper intermediate alloy CuP14 for deoxidation according to the phosphorus ratio, controlling the furnace temperature to 1150 ℃, keeping the temperature and standing for 15min, adding a tellurium-copper intermediate alloy CuTe, controlling the furnace temperature to 1250 ℃, keeping the temperature and standing for 15min, adding rare earth element scandium, stirring a molten pool after complete melting, adjusting the furnace temperature to 1200 ℃, baking a furnace end for multiple times, and then casting into ingots by water cooling;
(2) extruding: putting the copper alloy ingot obtained in the step (1) into an induction furnace, heating to 830 ℃, preserving heat for 30min to enable crystal grains to be uniformly refined, and then carrying out extrusion deformation processing; the extrusion deformation processing is carried out on an 800 horizontal extruder, the specification of the extrusion deformation processing is 1200+15KW, the extrusion adopts a reverse extrusion mode, the size of an extrusion die is 4.3mm by 40.3mm, and the extrusion temperature is 780 ℃ plus or minus 10 ℃;
(3) acid washing and hydraulic drawing: pickling the product obtained in the step (2), pickling the billet obtained after extrusion in a sulfuric acid tank with the concentration of 15%, washing off surface oxides, and then performing hydraulic drawing; the hydraulic drawing is carried out in a hydraulic drawing machine, the specification of the hydraulic drawing machine is 60+18KW, and the specification of a drawing die is phi 2.5mm and 39 mm;
(4) and polishing and sizing the section bar after the drawing deformation to obtain the finished product.
And (4) carrying out performance detection on the obtained tellurium-copper alloy, and averaging ten samples in each batch. The metal material tensile test refers to a standard GB/T228, the metal material bending test is carried out according to the standard GB/T232, and the detection method of the electric conductivity is carried out according to the regulation of a metal material resistivity measurement method GB/T351 standard. The mechanical properties of the obtained tellurium-copper alloy material are detected as follows: tensile strength Rm 382MPa, cutting performance 90%, elongation 22% and conductivity 97%.
Example 2
The tellurium-copper alloy material comprises the following elements in percentage by weight:
0.5 percent of Te; 0.12 percent of R; 0.005% of P; the balance of Cu; wherein R is rare earth element yttrium.
The preparation method of the tellurium-copper alloy material comprises the following steps:
(1) smelting: adding the rest cathode copper with the purity of 99.99 percent into a smelting furnace according to the corresponding weight percentage, and heating and melting under the covering protection of a covering agent (graphite flake); after cathode copper is completely melted, adding phosphorus-copper intermediate alloy CuP14 for deoxidation according to the phosphorus ratio, controlling the furnace temperature to 1170 ℃, keeping the temperature and standing, adding tellurium-copper intermediate alloy CuTe, controlling the furnace temperature to 1260 ℃, keeping the temperature and standing, adding rare earth element yttrium, stirring a molten pool after complete melting, adjusting the furnace temperature to 1240 ℃, baking the furnace end for multiple times, and then casting into ingots by water cooling;
(2) extruding: putting the copper alloy cast ingot obtained in the step (1) into an induction furnace, heating to 840 ℃, preserving heat for 45min to enable crystal grains to be uniformly refined, and then carrying out extrusion deformation processing; the extrusion deformation processing is carried out on an 800 horizontal extruder, the specification of the extrusion deformation processing is 1200+15KW, the extrusion adopts a reverse extrusion mode, the size of an extrusion die is 4.3mm by 40.3mm, and the extrusion temperature is 780 ℃ plus or minus 10 ℃;
(3) acid washing and hydraulic drawing: pickling the product obtained in the step (2), pickling the billet obtained after extrusion in a sulfuric acid tank with the concentration of 20%, washing off surface oxides, and then performing hydraulic drawing; the hydraulic drawing is carried out in a hydraulic drawing machine, the specification of the hydraulic drawing machine is 60+18KW, and the specification of a drawing die is phi 2.5mm and 39 mm;
(4) and polishing and sizing the section bar after the drawing deformation to obtain the finished product.
The performance of the tellurium copper alloy is detected according to the method of the embodiment 1, and the mechanical properties of the tellurium copper alloy material are detected as follows: the tensile strength Rm is 386MPa, the cutting performance is 92%, the elongation is 23% and the conductivity is 98%.
Example 3
The tellurium-copper alloy material comprises the following elements in percentage by weight:
0.35 percent of Te; r is 0.09 percent; p is 0.003 percent; the balance of Cu; wherein R is a mixture of rare earth elements scandium and yttrium (mass ratio is 1: 3).
The preparation method of the tellurium-copper alloy material comprises the following steps:
(1) smelting: adding the rest cathode copper with the purity of 99.99 percent into a smelting furnace according to the corresponding weight percentage, and heating and melting under the protection of covering agent (graphite powder); after cathode copper is completely melted, adding a phosphorus-copper intermediate alloy CuP14 for deoxidation according to the phosphorus ratio, controlling the furnace temperature to 1160 ℃, keeping the temperature and standing for 20min, adding a tellurium-copper intermediate alloy CuTe, controlling the furnace temperature to 1255 ℃, keeping the temperature and standing for 20min, adding a rare earth element R, stirring a molten pool after complete melting, adjusting the furnace temperature to 1220 ℃, baking a furnace end for multiple times, and then casting into ingots by water cooling;
(2) extruding: putting the copper alloy cast ingot obtained in the step (1) into an induction furnace, heating to 837 ℃, preserving heat for 40min to enable crystal grains to be uniformly refined, and then carrying out extrusion deformation processing; the extrusion deformation processing is carried out on an 800 horizontal extruder, the specification of the extrusion deformation processing is 1200+15KW, the extrusion adopts a reverse extrusion mode, the size of an extrusion die is 4.3mm by 40.3mm, and the extrusion temperature is 780 ℃ plus or minus 10 ℃;
(3) acid washing and hydraulic drawing: pickling the product obtained in the step (2), pickling the billet obtained after extrusion in a sulfuric acid tank with the concentration of 18%, washing off surface oxides, and then performing hydraulic drawing; the hydraulic drawing is carried out in a hydraulic drawing machine, the specification of the hydraulic drawing machine is 60+18KW, and the specification of a drawing die is phi 2.5mm and 39 mm;
(4) and polishing and sizing the section bar after the drawing deformation to obtain the finished product.
The performance of the tellurium copper alloy is detected according to the method of the embodiment 1, and the mechanical properties of the tellurium copper alloy material are detected as follows: the tensile strength Rm was 392MPa, the machinability was 94%, the elongation 24%, and the conductivity 98%.

Claims (8)

1. The preparation method of the tellurium-copper alloy material is characterized by comprising the following steps of: (1) smelting: adding the rest cathode copper with the purity of more than 99.99 percent into a smelting furnace according to the corresponding weight percentage, and heating and melting under the covering protection of a covering agent; after cathode copper is completely melted, adding a phosphor-copper intermediate alloy according to the proportion of phosphor to deoxidize, controlling the furnace temperature to 1150 ℃, keeping the temperature and standing, adding a tellurium-copper intermediate alloy CuTe, controlling the furnace temperature to 1250 ℃, keeping the temperature and standing, adding a rare earth element scandium, stirring a molten pool after complete melting, adjusting the furnace temperature to 1200 ℃, baking the furnace end for multiple times, and then casting into ingots by water cooling; (2) extruding: putting the copper alloy ingot obtained in the step (1) into an induction furnace, heating to 830 ℃, preserving heat for 30min to enable crystal grains to be uniformly refined, and then carrying out extrusion deformation processing; (3) acid washing and hydraulic drawing: performing acid washing on the product obtained in the step (2), washing off surface oxides, and then performing hydraulic drawing; the specification of the drawing die for hydraulic drawing is phi 2.5mm and 39 mm; (4) polishing and sizing the section bar after the drawing deformation to obtain the finished product; the tellurium-copper alloy material comprises the following elements in percentage by weight: te0.15 percent; 0.08 percent of R; 0.002% of P; the balance of Cu; r is rare earth element scandium.
2. The method for preparing the tellurium-copper alloy material as claimed in claim 1, wherein the covering agent in step (1) is one of charcoal, graphite flake or graphite powder.
3. The method for preparing the tellurium-copper alloy material as claimed in claim 1, wherein the phosphor-copper master alloy is CuP 14.
4. The method for preparing the tellurium-copper alloy material as claimed in claim 1, wherein the extrusion deformation processing is carried out on an 800 horizontal extruder, and the specification is 1200+15 kW.
5. The method for preparing the tellurium-copper alloy material as claimed in claim 4, wherein the extrusion is performed by backward extrusion at 780 ℃ ± 10 ℃.
6. The method for producing the tellurium-copper alloy material as claimed in claim 5, wherein the size of the extrusion die for the back extrusion is 4.3mm by 40.3 mm.
7. The method for preparing the tellurium-copper alloy material according to claim 1, wherein the acid washing is acid washing of the billet obtained after extrusion in a sulfuric acid bath with a concentration of 15-20%.
8. The method for preparing the tellurium-copper alloy material as claimed in claim 1, wherein the hydraulic drawing is performed in a hydraulic drawing machine with a specification of 60+18 kW.
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CN112458321B (en) * 2020-10-14 2021-11-09 陕西斯瑞新材料股份有限公司 Metal processing technology of tellurium-copper alloy wire for high-current electric connector
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CN115679146A (en) * 2022-10-28 2023-02-03 宁波金田铜业(集团)股份有限公司 Copper alloy and preparation method thereof
CN115786753B (en) * 2023-02-02 2023-05-30 泰州泰锦合金材料有限公司 Tellurium copper alloy material containing rare earth metal and preparation method thereof

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