CN113278826B - Preparation method of high-permeability copper-infiltrated wire - Google Patents

Preparation method of high-permeability copper-infiltrated wire Download PDF

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CN113278826B
CN113278826B CN202110547358.6A CN202110547358A CN113278826B CN 113278826 B CN113278826 B CN 113278826B CN 202110547358 A CN202110547358 A CN 202110547358A CN 113278826 B CN113278826 B CN 113278826B
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alloy
wire
copper
infiltrated
temperature
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CN113278826A (en
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周斌
田东松
郭创立
孙君鹏
王群
刘向东
苟锁
刘琦
梁相博
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Sirui Advanced Copper Alloy Co ltd
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Sirui Advanced Copper Alloy Co ltd
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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
    • C22C1/02—Making non-ferrous alloys by melting
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B21—MECHANICAL METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL; PUNCHING METAL
    • B21C—MANUFACTURE OF METAL SHEETS, WIRE, RODS, TUBES OR PROFILES, OTHERWISE THAN BY ROLLING; AUXILIARY OPERATIONS USED IN CONNECTION WITH METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL
    • B21C37/00—Manufacture of metal sheets, bars, wire, tubes or like semi-manufactured products, not otherwise provided for; Manufacture of tubes of special shape
    • B21C37/04—Manufacture of metal sheets, bars, wire, tubes or like semi-manufactured products, not otherwise provided for; Manufacture of tubes of special shape of bars or wire
    • B21C37/047—Manufacture of metal sheets, bars, wire, tubes or like semi-manufactured products, not otherwise provided for; Manufacture of tubes of special shape of bars or wire of fine wires
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22D—CASTING OF METALS; CASTING OF OTHER SUBSTANCES BY THE SAME PROCESSES OR DEVICES
    • B22D7/00—Casting ingots, e.g. from ferrous metals
    • B22D7/005—Casting ingots, e.g. from ferrous metals from non-ferrous metals
    • C—CHEMISTRY; METALLURGY
    • C21—METALLURGY OF IRON
    • C21D—MODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
    • C21D9/00—Heat treatment, e.g. annealing, hardening, quenching or tempering, adapted for particular articles; Furnaces therefor
    • C21D9/52—Heat treatment, e.g. annealing, hardening, quenching or tempering, adapted for particular articles; Furnaces therefor for wires; for strips ; for rods of unlimited length
    • C21D9/525—Heat treatment, e.g. annealing, hardening, quenching or tempering, adapted for particular articles; Furnaces therefor for wires; for strips ; for rods of unlimited length for wire, for rods
    • 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
    • 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
    • C22C9/04—Alloys based on copper with zinc 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

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  • Engineering & Computer Science (AREA)
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  • Metallurgy (AREA)
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  • Thermal Sciences (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Powder Metallurgy (AREA)

Abstract

The invention discloses a preparation method of a high-permeability copper-infiltrated wire material, which comprises S1, weighing Ni, Mn, Fe, Zn and Cu raw materials respectively, and mechanically mixing Ni, Mn, Fe, Zn and Cu to obtain a mixture; s2, placing the mixture into a vacuum smelting furnace for induction smelting to obtain an alloy solution; s3, pouring the alloy solution into a mold, cooling and demolding to obtain an alloy ingot; s4, heating, forging and turning the alloy ingot in an electric furnace to obtain an alloy bar; s5, hot rolling the alloy bar stock into a coiled round material; s6, drawing the coiled material into a coiled material; s7, cutting the alloy wire according to the required length; the method has reasonable process design, and the copper infiltrated wire prepared by the method has high permeability and low manufacturing cost, and is suitable for large-scale popularization.

Description

Preparation method of high-permeability copper-infiltrated wire
Technical Field
The invention relates to the technical field of metallurgical copper infiltration, in particular to a preparation method of a high-permeability copper infiltration wire.
Background
The powder metallurgy iron-based product is widely applied due to the characteristics of high material utilization rate, high size precision, few processing procedures and the like, and in the powder metallurgy iron-based product, the wear resistance and impact resistance of the powder metallurgy product can be obviously improved through a copper infiltration treatment process, and indexes such as strength, hardness and the like can be provided, so that the high-grade powder metallurgy iron-based product can be subjected to copper infiltration treatment when a green body is sintered.
However, the problems of low permeability, large density fluctuation, difficult residue cleaning and the like exist in the copper infiltration sintering in the current market, so that the mechanical property and the wear resistance are poor; in addition, the existing penetrant is mainly in a powder state, and the powder is easy to oxidize, high in production cost and complex in process in the water atomization preparation process, so that the development of high-end powder metallurgy preparation is limited to a great extent.
Disclosure of Invention
Aiming at the technical problems, the invention provides a preparation method of a high-permeability copper-infiltrated wire with low production cost.
The technical scheme of the invention is as follows: a preparation method of a high-permeability copper-infiltrated wire material comprises the following steps:
s1, preparing the ingredients
Weighing 0.05-0.5% of Ni, 0.1-1% of Mn, 1-3% of Fe, 1-5% of Zn and the balance of Cu according to weight percentage; then mechanically mixing Ni, Mn, Fe, Zn and Cu for 15-35min to obtain a mixture;
s2, vacuum melting
Placing the mixture obtained in the step S1 into a crucible of a vacuum melting furnace, and then pumping the vacuum degree in the vacuum melting furnace to 3 x 103Pa-6×103Pa, controlling the smelting current to be 1200-1600A, controlling the smelting power to be 5-8kW, then refining for 10-20min at the temperature of 1250-1280 ℃, and carrying out heat preservation treatment for 5-15min to obtain an alloy solution;
s3, casting and discharging
Cleaning the surface of the die, wherein no impurities or oil stains are attached, preheating a pouring channel embedded with a ceramic filter plate to 1100-1300 ℃, pouring the alloy solution obtained in the step S2 into the pouring channel, adsorbing and filtering the impurities in the alloy solution by the ceramic filter plate, then feeding the impurities into the die, cooling, and demoulding to obtain an alloy ingot; wherein, in the casting process, the casting speed is firstly slow, then fast and finally slow;
s4, hot forging and turning outer circle
Heating the alloy ingot obtained in the step S3 to 910-950 ℃ in an electric furnace, preserving heat for 2-3h, then placing the alloy ingot into a forging die for forging to form a bar with the diameter of phi 30-40mm, and finally turning to remove oxide skin on the surface of the bar to obtain an alloy bar;
s5, hot rolling and coiling
The alloy bar obtained in the step S4 is heated to 850-880 ℃, the temperature is kept for 0.5-1.2h, the alloy bar is rolled into a primary alloy wire with phi 8-12mm on a planetary rolling mill at a hot rolling speed of 50-80m/min, and then the primary alloy wire is placed on a wire rod coiling machine and can be coiled into a wire rod material with 15-45 m/coil;
s6, drawing and annealing
Carrying out multi-pass drawing on the disc material obtained in the step S5 on a disc drawing machine, controlling the drawing speed to be 0.5-2.5m/min, controlling the single-pass processing deformation rate to be 4-8%, obtaining a copper-infiltrated wire material with the diameter of 1-3mm after finishing drawing, and carrying out annealing treatment on the copper-infiltrated wire material at the temperature of 500-550 ℃ in the drawing process;
s7, cutting
And cutting the alloy wire obtained in the step S6 according to the required length.
Further, after the step S1 is completed, the mixture is sent into a hydrogen reduction furnace for diffusion, the diffusion temperature is controlled to be 300-.
Further, after the step S2 is completed, the temperature of the alloy solution is firstly raised to 1050 ℃ C. of 850-.
Further, after the step S3 is completed, the alloy ingot is placed in a graphite boat, the feeding copper accounting for 5-8% of the mass of the alloy ingot is added, then sintering treatment is carried out at the temperature of 1200-1500 ℃, and the feeding copper is added into the alloy ingot, so that the surface quality and the forming effect of the formed copper infiltrated wire can be improved.
Further, in step S6, uniformly coating a lubricant before drawing the wire rod, wherein the lubricant is composed of mineral oil, graphene and deionized water according to a volume ratio of 1:2: 1; by smearing the lubricant, the friction between the wire rod and the wire drawing machine in the drawing process can be reduced, and the surface quality of the copper-infiltrated wire material after drawing forming is improved.
Further, in step S6, the annealing treatment includes an open fire heating stage and a high temperature tempering stage, wherein the temperature of the open fire heating stage is 500-; the temperature of the high-temperature tempering stage is 525-550 ℃, and the time is 15-30 min; by carrying out open fire heating and high-temperature tempering treatment on the copper infiltrated wire, the internal stress of the wire in the drawing process can be reduced, the breakage phenomenon of the wire in the drawing process is avoided, and the mechanical property of the formed copper infiltrated wire is improved.
Further, after the step S4 is completed, the alloy bar is put into an electric furnace, the temperature is raised to 800-.
Further, after the step S6 is finished, soaking the copper infiltrated wire material in 12% by mass of HCl aqueous solution for 5-25min, taking out, washing with deionized water for 3-5 times, and naturally drying; the oxidation resistance of the copper infiltrated wire can be improved by carrying out acid washing on the copper infiltrated wire.
Further, after the step S7 is finished, the copper infiltrated wire after cutting and cutting is placed into a shaping furnace, and shaping treatment is carried out for 50-110min under the helium atmosphere and at the temperature of 180-350 ℃; through the sizing treatment of the copper infiltrated wire, the tensile strength and elasticity of the copper infiltrated wire can be obviously improved, and the using effect of the copper infiltrated wire is improved.
Compared with the prior art, the invention has the beneficial effects that: the process structure of the invention is reasonable in design, and the high-infiltration rate copper infiltrated material provided by the invention is utilized and prepared into a wire material form, so that the infiltration rate is improved, and the production cost is lower; the copper infiltrated wire prepared by the method improves the density and the copper infiltrated depth of the iron-based copper infiltrated product, has high permeability, uniform density of the copper infiltrated iron base and no residue, thereby improving the overall performance of the product and having wide application prospect; according to the technical scheme, the raw materials are subjected to diffusion treatment after the raw materials are mixed, so that the erosion of the prepared copper infiltrated wire to an infiltration base material is reduced, the forming effect and the copper infiltration depth of a workpiece are improved, and the uniformity of crystal grains in the tissue of the finished copper infiltrated wire is improved due to the heating and heat preservation treatment of the alloy solution, so that the deformation resistance of the internal tissue of the copper infiltrated wire in a high-temperature state is improved; because the feeding copper is added into the alloy cast ingot, the surface quality and the forming effect of the copper infiltrated wire after forming can be improved; because open fire heating and high-temperature tempering are carried out on the copper infiltrated wire, the internal stress of the wire in the drawing process can be reduced, the breakage phenomenon of the wire in the drawing process is avoided, and the mechanical property of the formed copper infiltrated wire is improved; the oxidation resistance of the copper infiltrated wire can be improved by pickling the copper infiltrated wire; by carrying out shaping treatment on the copper infiltrated wire, the tensile strength and elasticity of the copper infiltrated wire can be obviously improved, and the using effect of the copper infiltrated wire is improved; because the alloy bar is heated and quenched, the stored energy generated by the alloy bar in the hot forging process can be slowly released, the expansion of internal crystal grains of the alloy bar in the quenching process is avoided, the uniformity of internal tissues of the alloy bar is improved, and the quality of the copper infiltrated wire is further improved.
Drawings
FIG. 1 is a schematic diagram showing the appearance of a copper-infiltrated wire prepared according to the present invention.
Detailed Description
Example 1: a preparation method of a high-permeability copper-infiltrated wire material comprises the following steps:
s1, preparing the ingredients
Weighing 0.05 percent of Ni, 0.1 percent of Mn, 1 percent of Fe, 1 percent of Zn and the balance of Cu according to the weight percentage; then mechanically mixing Ni, Mn, Fe, Zn and Cu for 15min to obtain a mixture;
s2, vacuum melting
Placing the mixture obtained in the step S1 into a crucible of a vacuum melting furnace, and then pumping the vacuum degree in the vacuum melting furnace to 3 x 103Pa, controlling the smelting current to be 1200A and the smelting power to be 5kW, then refining for 10min at the temperature of 1250 ℃, and carrying out heat preservation treatment for 5min to obtain an alloy solution;
s3, casting and discharging
Cleaning the surface of the die, removing impurities and oil stains, preheating a pouring channel embedded with a ceramic filter plate to 1100 ℃, pouring the alloy solution obtained in the step S2 into the pouring channel, adsorbing and filtering the impurities in the alloy solution by the ceramic filter plate, then feeding the filtered impurities into the die, cooling and demoulding to obtain an alloy ingot; wherein, in the casting process, the casting speed is firstly slow, then fast and finally slow;
s4, hot forging and turning outer circle
Heating the alloy cast ingot obtained in the step S3 to 910 ℃ in an electric furnace, preserving heat for 2h, then placing the alloy cast ingot into a forging die for forging to form a bar with the diameter of phi 30mm, and finally turning to remove oxide skin on the surface of the bar to obtain an alloy bar;
s5, hot rolling and coiling
Heating the alloy bar obtained in the step S4 to 850 ℃ again, keeping the temperature for 0.5h, rolling the alloy bar into a primary alloy wire with the diameter of 8mm on a planetary rolling mill at the hot rolling speed of 50m/min, and then placing the primary alloy wire on a coiling machine to coil into a coiled material with the diameter of 15 m/coil;
s6, drawing and annealing
Carrying out multi-pass drawing on the disc material obtained in the step S5 on a disc drawing machine, controlling the drawing speed to be 0.5m/min and the single-pass processing deformation rate to be 4%, obtaining a copper-infiltrated wire material with the diameter of phi 1mm after drawing is finished, and annealing the copper-infiltrated wire material at the temperature of 500 ℃ in the drawing process;
s7, cutting
And cutting the alloy wire obtained in the step S6 according to the required length.
Example 2: a preparation method of a high-permeability copper-infiltrated wire material comprises the following steps:
s1, preparing the ingredients
Weighing 0.25 percent of Ni, 0.5 percent of Mn, 2 percent of Fe, 3 percent of Zn and the balance of Cu according to the weight percentage; then mechanically mixing Ni, Mn, Fe, Zn and Cu for 20min to obtain a mixture; the mixture is sent into a hydrogen reduction furnace for diffusion, the diffusion temperature is controlled to be 300 ℃, the diffusion time is 50min, and the mixture is subjected to diffusion treatment, so that the erosion of the prepared copper-infiltrated wire to an infiltration base material is reduced, and the forming effect and the copper infiltration depth of a workpiece are improved;
s2, vacuum melting
Placing the mixture obtained in the step S1 into a crucible of a vacuum melting furnace, and then pumping the vacuum degree in the vacuum melting furnace to 5 multiplied by 103Pa, controlling the smelting current to 1400A and the smelting power to 6kW, then refining for 15min at the temperature of 1265 ℃, and carrying out heat preservation treatment for 10min to obtain an alloy solution;
s3, casting and discharging
Cleaning the surface of the die, removing impurities and oil stains, preheating a pouring channel embedded with a ceramic filter plate to 1220 ℃, pouring the alloy solution obtained in the step S2 into the pouring channel, adsorbing and filtering the impurities in the alloy solution by the ceramic filter plate, then feeding the filtered impurities into the die, cooling and demoulding to obtain an alloy ingot; wherein, in the casting process, the casting speed is firstly slow, then fast and finally slow;
s4, hot forging and turning outer circle
Heating the alloy cast ingot obtained in the step S3 to 935 ℃ in an electric furnace, preserving heat for 3h, then placing the alloy cast ingot into a forging die for forging to form a bar with the diameter of phi 35mm, and finally turning to remove oxide skin on the surface of the bar to obtain an alloy bar;
s5, hot rolling and coiling
Heating the alloy bar stock obtained in the step S4 to 865 ℃, preserving heat for 0.8h, rolling the alloy bar stock on a planetary rolling mill at a hot rolling speed of 65mm/min to obtain a primary alloy wire with the diameter of 10mm, and then placing the primary alloy wire on a coiling machine to coil into a coiled material with the coil diameter of 30 m/coil;
s6, drawing and annealing
Carrying out multi-pass drawing on the disc material obtained in the step S5 on a disc drawing machine, controlling the drawing speed to be 1.5m/min and the single-pass processing deformation rate to be 6%, obtaining a copper-infiltrated wire material with phi of 2mm after drawing is finished, and annealing the copper-infiltrated wire material at 525 ℃ in the drawing process; uniformly coating a lubricant before drawing the coiled material, wherein the lubricant consists of mineral oil, graphene and deionized water according to a volume ratio of 1:2: 1; by smearing the lubricant, the friction between the wire rod and the wire drawing machine in the drawing process can be reduced, and the surface quality of the copper-infiltrated wire material after drawing forming is improved.
S7, cutting
And cutting the alloy wire obtained in the step S6 according to the required length.
Example 3: a preparation method of a high-permeability copper-infiltrated wire material comprises the following steps:
s1, preparing the ingredients
Weighing 0.5 percent of Ni, 1 percent of Mn, 3 percent of Fe, 5 percent of Zn and the balance of Cu according to the weight percentage; then mechanically mixing Ni, Mn, Fe, Zn and Cu for 35min to obtain a mixture;
s2, vacuum melting
Placing the mixture obtained in the step S1 into a crucible of a vacuum melting furnace, and then pumping the vacuum degree in the vacuum melting furnace to 6 x 103Pa, controlling the smelting current to be 1600A and the smelting power to be 8kW, then refining at the temperature of 1280 ℃ for 20min, and carrying out heat preservation treatment for 15min to obtain an alloy solution; the alloy solution is heated to 850 ℃ firstly, the heat preservation treatment is carried out for 15min, then the temperature is heated to 1050 ℃, the heat preservation treatment is carried out for 10min, and finally the temperature is increased to 300 ℃ at the speed of 8 ℃/min;
s3, casting and discharging
Cleaning the surface of the die, removing impurities and oil stains, preheating a pouring channel embedded with a ceramic filter plate to 1300 ℃, pouring the alloy solution obtained in the step S2 into the pouring channel, adsorbing and filtering the impurities in the alloy solution by the ceramic filter plate, then feeding the impurity solution into the die, cooling and demoulding to obtain an alloy ingot; wherein, in the casting process, the casting speed is firstly slow, then fast and finally slow;
s4, hot forging and turning outer circle
Heating the alloy cast ingot obtained in the step S3 to 950 ℃ in an electric furnace, preserving heat for 3 hours, then placing the alloy cast ingot into a forging die for forging to form a bar with the diameter of 40mm, and finally turning to remove oxide skin on the surface of the bar to obtain an alloy bar;
s5, hot rolling and coiling
Heating the alloy bar obtained in the step S4 to 880 ℃ again, preserving heat for 1.2h, rolling the alloy bar into a primary alloy wire with the diameter of 12mm on a planetary rolling mill at the hot rolling speed of 80mm/min, and then placing the primary alloy wire on a coiling machine to coil into a coiling material with the coil diameter of 45 m/coil;
s6, drawing and annealing
Carrying out multi-pass drawing on the disc material obtained in the step S5 on a disc drawing machine, controlling the drawing speed to be 2.5m/min and the single-pass processing deformation rate to be 8%, obtaining a copper-infiltrated wire material with the diameter of phi 3mm after drawing is finished, and annealing the copper-infiltrated wire material at 550 ℃ in the drawing process;
s7, cutting
And cutting the alloy wire obtained in the step S6 according to the required length.
Example 4: a preparation method of a high-permeability copper-infiltrated wire material comprises the following steps:
s1, preparing the ingredients
Weighing 0.05 percent of Ni, 0.1 percent of Mn, 1 percent of Fe, 1 percent of Zn and the balance of Cu according to the weight percentage; then mechanically mixing Ni, Mn, Fe, Zn and Cu for 20min to obtain a mixture;
s2, vacuum melting
Placing the mixture obtained in the step S1 into a crucible of a vacuum melting furnace, and then pumping the vacuum degree in the vacuum melting furnace to 3 x 103Pa, controlling the smelting current to be 1200A, and smeltingRefining at 5kW, refining at 1250 ℃ for 10min, and carrying out heat preservation treatment for 5min to obtain an alloy solution;
s3, casting and discharging
Cleaning the surface of the die, removing impurities and oil stains, preheating a pouring channel embedded with a ceramic filter plate to 1100 ℃, pouring the alloy solution obtained in the step S2 into the pouring channel, adsorbing and filtering the impurities in the alloy solution by the ceramic filter plate, then feeding the filtered impurities into the die, cooling and demoulding to obtain an alloy ingot; wherein, in the casting process, the casting speed is firstly slow, then fast and finally slow; placing the alloy ingot in a graphite boat, adding feeding copper accounting for 5% of the mass of the alloy ingot, sintering at 1200 ℃, and adding the feeding copper into the alloy ingot, so that the surface quality and the forming effect of the formed copper-infiltrated wire can be improved;
s4, hot forging and turning outer circle
Heating the alloy cast ingot obtained in the step S3 to 910 ℃ in an electric furnace, preserving heat for 2h, then placing the alloy cast ingot into a forging die for forging to form a bar with the diameter of phi 30mm, and finally turning to remove oxide skin on the surface of the bar to obtain an alloy bar;
s5, hot rolling and coiling
Heating the alloy bar obtained in the step S4 to 850 ℃ again, keeping the temperature for 0.5h, rolling the alloy bar into a primary alloy wire with the diameter of 8mm on a planetary rolling mill at the hot rolling speed of 50mm/min, and then placing the primary alloy wire on a coiling machine to coil into a coiled material with the coil diameter of 15 m/coil;
s6, drawing and annealing
Carrying out multi-pass drawing on the disc material obtained in the step S5 on a disc drawing machine, controlling the drawing speed to be 0.5m/min and the single-pass processing deformation rate to be 4%, obtaining a copper-infiltrated wire material with the diameter of phi 1mm after drawing is finished, and annealing the copper-infiltrated wire material at the temperature of 500 ℃ in the drawing process;
s7, cutting
And cutting the alloy wire obtained in the step S6 according to the required length.
Example 5: a preparation method of a high-permeability copper-infiltrated wire material comprises the following steps:
s1, preparing the ingredients
Weighing 0.5 percent of Ni, 1 percent of Mn, 3 percent of Fe, 5 percent of Zn and the balance of Cu according to the weight percentage; then mechanically mixing Ni, Mn, Fe, Zn and Cu for 35min to obtain a mixture;
s2, vacuum melting
Placing the mixture obtained in the step S1 into a crucible of a vacuum melting furnace, and then pumping the vacuum degree in the vacuum melting furnace to 6 x 103Pa, controlling the smelting current to be 1600A and the smelting power to be 8kW, then refining at the temperature of 1280 ℃ for 20min, and carrying out heat preservation treatment for 15min to obtain an alloy solution;
s3, casting and discharging
Cleaning the surface of the die, removing impurities and oil stains, preheating a pouring channel embedded with a ceramic filter plate to 1300 ℃, pouring the alloy solution obtained in the step S2 into the pouring channel, adsorbing and filtering the impurities in the alloy solution by the ceramic filter plate, then feeding the impurity solution into the die, cooling and demoulding to obtain an alloy ingot; wherein, in the casting process, the casting speed is firstly slow, then fast and finally slow;
s4, hot forging and turning outer circle
Heating the alloy cast ingot obtained in the step S3 to 950 ℃ in an electric furnace, preserving heat for 3 hours, then placing the alloy cast ingot into a forging die for forging to form a bar with the diameter of 40mm, and finally turning to remove oxide skin on the surface of the bar to obtain an alloy bar;
s5, hot rolling and coiling
Heating the alloy bar obtained in the step S4 to 880 ℃ again, preserving heat for 1.2h, rolling the alloy bar into a primary alloy wire with the diameter of 8mm on a planetary rolling mill at the hot rolling speed of 80mm/min, and then placing the primary alloy wire on a coiling machine to coil into a coiling material with the coil diameter of 45 m/coil;
s6, drawing and annealing
Carrying out multi-pass drawing on the disc material obtained in the step S5 on a disc drawing machine, controlling the drawing speed to be 2.5m/min and the single-pass processing deformation rate to be 8%, obtaining a copper-infiltrated wire material with the diameter of phi 3mm after drawing is finished, and annealing the copper-infiltrated wire material at 550 ℃ in the drawing process; uniformly coating a lubricant before drawing the coiled material, wherein the lubricant consists of mineral oil, graphene and deionized water according to a volume ratio of 1:2: 1; by smearing the lubricant, the friction between the wire rod and a wire drawing machine in the drawing process of the wire rod can be reduced, and the surface quality of the copper-infiltrated wire material after drawing forming is improved; the annealing treatment comprises an open fire heating stage and a high temperature tempering stage, wherein the temperature of the open fire heating stage is 500 ℃, and the time is 20 min; the temperature of the high-temperature tempering stage is 525 ℃ and the time is 15 min; by carrying out open fire heating and high-temperature tempering treatment on the copper infiltrated wire, the internal stress of the wire in the drawing process can be reduced, the breakage phenomenon of the wire in the drawing process is avoided, and the mechanical property of the formed copper infiltrated wire is improved; finally, soaking the copper infiltrated wire in 12% by mass of HCl aqueous solution for 5min, taking out, washing with deionized water for 3 times, and naturally drying; the oxidation resistance of the copper infiltrated wire can be improved by pickling the copper infiltrated wire;
s7, cutting
Cutting the alloy wire material obtained in the step S6 according to the required length, putting the cut copper infiltrated wire material into a shaping furnace, and shaping for 50min at the temperature of 180 ℃ in the helium atmosphere; through the sizing treatment of the copper infiltrated wire, the tensile strength and elasticity of the copper infiltrated wire can be obviously improved, and the using effect of the copper infiltrated wire is improved.
Example 6: a preparation method of a high-permeability copper-infiltrated wire material comprises the following steps:
s1, preparing the ingredients
Weighing 0.05 percent of Ni, 0.1 percent of Mn, 1 percent of Fe, 1 percent of Zn and the balance of Cu according to the weight percentage; then mechanically mixing Ni, Mn, Fe, Zn and Cu for 35min to obtain a mixture;
s2, vacuum melting
Placing the mixture obtained in the step S1 into a crucible of a vacuum melting furnace, and then pumping the vacuum degree in the vacuum melting furnace to 3 x 103Pa, controlling the smelting current to be 1200A and the smelting power to be 5kW, then refining for 10min at the temperature of 1250 ℃, and carrying out heat preservation treatment for 5min to obtain an alloy solution;
s3, casting and discharging
Cleaning the surface of the die, removing impurities and oil stains, preheating a pouring channel embedded with a ceramic filter plate to 1100 ℃, pouring the alloy solution obtained in the step S2 into the pouring channel, adsorbing and filtering the impurities in the alloy solution by ceramic, then feeding the alloy solution into the die, cooling and demoulding to obtain an alloy ingot; wherein, in the casting process, the casting speed is firstly slow, then fast and finally slow;
s4, hot forging and turning outer circle
Heating the alloy cast ingot obtained in the step S3 to 910 ℃ in an electric furnace, preserving heat for 2h, then placing the alloy cast ingot into a forging die for forging to form a bar with the diameter of phi 30mm, and finally turning to remove oxide skin on the surface of the bar to obtain an alloy bar; putting the alloy bar into an electric furnace, heating to 800 ℃ at a heating rate of 50 ℃/h, preserving heat for 4h, then quenching to 270 ℃ in purified water at the temperature of 30 ℃, naturally cooling to room temperature after discharging, and slowly releasing stored energy generated in the hot forging process of the alloy bar through the operation, so that internal crystal grain expansion of the alloy bar in the quenching process is avoided, the uniformity of internal tissues of the alloy bar is improved, and the quality of the copper-infiltrated wire is further improved;
s5, hot rolling and coiling
Heating the alloy bar obtained in the step S4 to 850 ℃ again, keeping the temperature for 0.5h, rolling the alloy bar into a primary alloy wire with the diameter of 8mm on a planetary rolling mill at the hot rolling speed of 5mm/min, and then placing the primary alloy wire on a coiling machine to coil into a coiled material with the diameter of 15 m/coil;
s6, drawing and annealing
Carrying out multi-pass drawing on the disc material obtained in the step S5 on a disc drawing machine, controlling the drawing speed to be 0.5m/min and the single-pass processing deformation rate to be 4%, obtaining a copper-infiltrated wire material with the diameter of phi 1mm after drawing is finished, and annealing the copper-infiltrated wire material at the temperature of 500 ℃ in the drawing process;
s7, cutting
And cutting the alloy wire obtained in the step S6 according to the required length.
Example 7: a preparation method of a high-permeability copper-infiltrated wire material comprises the following steps:
s1, preparing the ingredients
Weighing 0.25 percent of Ni, 0.5 percent of Mn, 2 percent of Fe, 3 percent of Zn and the balance of Cu according to the weight percentage; then mechanically mixing Ni, Mn, Fe, Zn and Cu for 35min to obtain a mixture; the mixture is sent into a hydrogen reduction furnace for diffusion, the diffusion temperature is controlled to be 500 ℃, the diffusion time is 80min, the corrosion of the prepared copper-infiltrated wire to an infiltration base material is reduced by performing diffusion treatment on the mixture, and the forming effect and the copper infiltration depth of a workpiece are improved;
s2, vacuum melting
Placing the mixture obtained in the step S1 into a crucible of a vacuum melting furnace, and then pumping the vacuum degree in the vacuum melting furnace to 6 x 103Pa, controlling the smelting current to be 1600A and the smelting power to be 8kW, then refining at the temperature of 1280 ℃ for 20min, and carrying out heat preservation treatment for 15min to obtain an alloy solution; the alloy solution is heated to 1050 ℃ firstly, the heat preservation treatment is carried out for 34min, then the temperature is heated to 1350 ℃, the heat preservation treatment is carried out for 30min, and finally the temperature is increased to 500 ℃ at the speed of 25 ℃/min;
s3, casting and discharging
Cleaning the surface of the die, removing impurities and oil stains, preheating a pouring channel embedded with a ceramic filter plate to 1300 ℃, pouring the alloy solution obtained in the step S2 into the pouring channel, allowing the impurities in the alloy solution to be adsorbed and filtered by the ceramic and then enter the die, cooling and demoulding to obtain an alloy ingot; wherein, in the casting process, the casting speed is firstly slow, then fast and finally slow; placing the alloy cast ingot in a graphite boat, adding feeding copper accounting for 8% of the mass of the alloy cast ingot, sintering at 1500 ℃, and adding the feeding copper into the alloy cast ingot, so that the surface quality and the forming effect of the formed copper-infiltrated wire can be improved;
s4, hot forging and turning outer circle
Heating the alloy cast ingot obtained in the step S3 to 950 ℃ in an electric furnace, preserving heat for 3 hours, then placing the alloy cast ingot into a forging die for forging to form a bar with the diameter of 40mm, and finally turning to remove oxide skin on the surface of the bar to obtain an alloy bar; putting the alloy bar into an electric furnace, heating to 1150 ℃ at the heating rate of 115 ℃/h, preserving heat for 5h, then quenching to 350 ℃ in purified water at the temperature of 60 ℃, naturally cooling to room temperature after discharging, and slowly releasing stored energy generated in the hot forging process of the alloy bar through the operation, thereby avoiding the expansion of internal crystal grains of the alloy bar in the quenching process, improving the uniformity of internal tissues of the alloy bar and further improving the quality of the copper-infiltrated wire;
s5, hot rolling and coiling
Heating the alloy bar obtained in the step S4 to 880 ℃ again, preserving heat for 1.2h, rolling the alloy bar into a primary alloy wire with the diameter of 8mm on a planetary rolling mill at a hot rolling speed of 66mm/min, and then placing the primary alloy wire on a coiling machine to coil into a coiled material with the coil diameter of 30 m/coil;
s6, drawing and annealing
Carrying out multi-pass drawing on the disc material obtained in the step S5 on a disc drawing machine, controlling the drawing speed to be 1.2m/min and the single-pass processing deformation rate to be 6%, obtaining a copper-infiltrated wire material with the diameter of 1mm after drawing is finished, and annealing the copper-infiltrated wire material at 550 ℃ in the drawing process; uniformly coating a lubricant before drawing the coiled material, wherein the lubricant consists of mineral oil, graphene and deionized water according to a volume ratio of 1:2: 1; by smearing the lubricant, the friction between the wire rod and a wire drawing machine in the drawing process of the wire rod can be reduced, and the surface quality of the copper-infiltrated wire material after drawing forming is improved; the annealing treatment comprises an open fire heating stage and a high temperature tempering stage, wherein the temperature of the open fire heating stage is 525 ℃, and the time is 45 min; the temperature of the high-temperature tempering stage is 550 ℃, and the time is 30 min; by carrying out open fire heating and high-temperature tempering treatment on the copper infiltrated wire, the internal stress of the wire in the drawing process can be reduced, the breakage phenomenon of the wire in the drawing process is avoided, and the mechanical property of the formed copper infiltrated wire is improved; soaking the copper infiltrated wire in 12% by mass of HCl aqueous solution for 25min, taking out, washing with deionized water for 5 times, and naturally drying; the oxidation resistance of the copper infiltrated wire can be improved by pickling the copper infiltrated wire;
s7, cutting
Cutting the alloy wire obtained in the step S6 according to the required length; putting the cut copper infiltrated wire into a shaping furnace, and shaping for 110min at the temperature of 350 ℃ in a helium atmosphere; through the sizing treatment of the copper infiltrated wire, the tensile strength and elasticity of the copper infiltrated wire can be obviously improved, and the using effect of the copper infiltrated wire is improved.
Test example: the performance tests of the copper infiltrated wire materials obtained in the embodiments 1 to 7 of the invention are respectively carried out, and the test results are shown in Table 1:
table 1, performance test results of the copper infiltrated wire under different conditions;
Figure GDA0003387259530000141
as can be seen from the comparison of the data in the table 1, in the example 2, compared with the example 1, because the diffusion treatment is carried out after the raw materials are mixed, and the lubricant is uniformly coated before the wire rod is drawn, the corrosion of the prepared copper infiltrated wire to the infiltration base material is reduced, the forming effect and the copper infiltration depth of the workpiece are improved, and the surface quality of the copper infiltrated wire after the drawing forming is also improved; compared with the embodiment 1, the temperature rise and the heat preservation treatment are carried out on the alloy solution, so that the grain uniformity of the finished product copper infiltrated wire tissue is improved, and the internal tissue anti-deformation capability of the copper infiltrated wire in a high-temperature state is further improved; example 4 compared with example 1, the surface quality and the forming effect of the copper infiltrated wire after forming can be improved due to the addition of the feeding copper into the alloy ingot; compared with the embodiment 1, the embodiment 5 has the advantages that as the copper infiltrated wire is subjected to open flame heating and high-temperature tempering treatment, the internal stress of the wire in the drawing process can be reduced, the breakage phenomenon of the wire in the drawing process is avoided, and the mechanical property of the formed copper infiltrated wire is improved; the oxidation resistance of the copper infiltrated wire can be improved by pickling the copper infiltrated wire; by carrying out shaping treatment on the copper infiltrated wire, the tensile strength and elasticity of the copper infiltrated wire can be obviously improved, and the using effect of the copper infiltrated wire is improved; compared with the embodiment 1, the embodiment 6 has the advantages that the alloy bar is heated and quenched, so that the stored energy generated by the alloy bar in the hot forging process can be slowly released, the internal crystal grains of the alloy bar are prevented from expanding in the quenching process, the uniformity of the internal structure of the alloy bar is improved, and the quality of the copper-infiltrated wire is further improved; example 7 compared with examples 1, 2, 3, 4, 5 and 6, the physical properties of the copper infiltrated wire material are further improved due to the combination of favorable conditions.

Claims (1)

1. A preparation method of a high-permeability copper-infiltrated wire is characterized by comprising the following steps:
s1, preparing the ingredients
Weighing 0.05-0.5% of Ni, 0.1-1% of Mn, 1-3% of Fe, 1-5% of Zn and the balance of Cu according to weight percentage; then mechanically mixing the Ni, Mn, Fe, Zn and Cu for 15-35min to obtain a mixture;
s2, vacuum melting
Placing the mixture obtained in the step S1 into a crucible of a vacuum melting furnace, and then pumping the vacuum degree in the vacuum melting furnace to 3 x 103Pa-6×103Pa, controlling the smelting current to be 1200-1600A, controlling the smelting power to be 5-8kW, then refining for 10-20min at the temperature of 1250-1280 ℃, and carrying out heat preservation treatment for 5-15min to obtain an alloy solution;
s3, casting and discharging
Cleaning the surface of the die, wherein no impurities or oil stains are attached, preheating a pouring channel embedded with a ceramic filter plate to 1100-1300 ℃, pouring the alloy solution obtained in the step S2 into the pouring channel, adsorbing and filtering the impurities in the alloy solution by the ceramic filter plate, then feeding the impurities into the die, cooling, and demoulding to obtain an alloy ingot; wherein, in the casting process, the casting speed is firstly slow, then fast and finally slow;
s4, hot forging and turning outer circle
Heating the alloy ingot obtained in the step S3 to 910-950 ℃ in an electric furnace, preserving heat for 2-3h, then placing the alloy ingot into a forging die for forging to form a bar with the diameter of phi 30-40mm, and finally turning to remove oxide skin on the surface of the bar to obtain an alloy bar;
s5, hot rolling and coiling
The alloy bar obtained in the step S4 is heated to 850-880 ℃, after heat preservation for 0.5-1.2h, the alloy bar is rolled into a primary alloy wire with phi 8-12mm on a planetary rolling mill at a hot rolling speed of 50-80m/min, and then the primary alloy wire is placed on a wire rod coiling machine and can be coiled into a wire rod material with 15-45 m/coil;
s6, drawing and annealing
Carrying out multi-pass drawing on the disc material obtained in the step S5 on a disc drawing machine, controlling the drawing speed to be 0.5-2.5m/min, controlling the single-pass processing deformation rate to be 4-8%, obtaining a copper-infiltrated wire material with the diameter of 1-3mm after finishing drawing, and carrying out annealing treatment on the copper-infiltrated wire material at the temperature of 500-550 ℃ in the drawing process;
s7, cutting
Cutting the alloy wire obtained in the step S6 according to the required length;
after the step S1 is finished, the mixture is sent into a hydrogen reduction furnace for diffusion, the diffusion temperature is controlled to be 300-;
after the step S2 is finished, the temperature of the alloy solution is firstly raised to 1050 ℃ of 850-;
after the step S3 is finished, the alloy ingot is placed in a graphite boat, feeding copper accounting for 5-8% of the mass of the alloy ingot is added, and then sintering treatment is carried out at the temperature of 1200-1500 ℃;
in the step S6, uniformly coating a lubricant before drawing the disc material, wherein the lubricant is composed of mineral oil, graphene and deionized water according to a volume ratio of 1:2: 1;
in step S6, the annealing treatment comprises an open fire heating stage and a high temperature tempering stage, wherein the temperature of the open fire heating stage is 500-525 ℃, and the time is 20-45 min; the temperature of the high-temperature tempering stage is 525-550 ℃, and the time is 15-30 min;
after the step S4 is finished, the alloy bar is put into an electric furnace, the temperature is raised to 1150 ℃ at the heating rate of 50-115 ℃/h, the temperature is kept for 4-5h, then the alloy bar is quenched in purified water at the temperature of 30-60 ℃ to 350 ℃ at 270 ℃ and naturally cooled to the room temperature after being taken out of the furnace;
after the step S6 is finished, soaking the copper infiltrated wire material in 12% by mass of HCl aqueous solution for 5-25min, taking out, washing with deionized water for 3-5 times, and naturally drying;
and step S7, after the step S7 is finished, the cut copper infiltrated wire material is placed into a shaping furnace, and shaping treatment is carried out for 50-110min under the helium atmosphere and the temperature condition of 180-350 ℃.
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