CN110564987B - High-strength and high-conductivity magnetic-compatibility copper alloy and preparation method of strip thereof - Google Patents

High-strength and high-conductivity magnetic-compatibility copper alloy and preparation method of strip thereof Download PDF

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CN110564987B
CN110564987B CN201910822511.4A CN201910822511A CN110564987B CN 110564987 B CN110564987 B CN 110564987B CN 201910822511 A CN201910822511 A CN 201910822511A CN 110564987 B CN110564987 B CN 110564987B
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CN110564987A (en
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曾力维
王永如
李正
傅新欣
巢国辉
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Ningbo Jintian Copper Group Co Ltd
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    • 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
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    • B22—CASTING; POWDER METALLURGY
    • B22D—CASTING OF METALS; CASTING OF OTHER SUBSTANCES BY THE SAME PROCESSES OR DEVICES
    • B22D11/00—Continuous casting of metals, i.e. casting in indefinite lengths
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    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
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    • C22C9/00—Alloys based on copper
    • 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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Abstract

High-strength and high-conductivity magnetic compatible copper alloy and a preparation method of a strip thereof. A high-strength and high-conductivity magnetic compatible copper alloy is characterized in that: the copper alloy comprises the following components in percentage by weight: fe: 5-6%, Ni: 0.01-2%, Si: 0.01-0.5%, Co: 0 to 0.1%, Nb: 0.007-0.012%, C: 0.01 to 0.1% by weight, and the balance copper and inevitable trace impurities. The preparation method comprises the following steps: material preparation and smelting: semi-continuous casting; hot rolling and online solid solution; milling, rough rolling and trimming; step aging; cleaning and finish rolling; stress relief annealing of the finished product; cleaning, splitting finished products and packaging. The preparation process is reasonable, the formula is scientific and reasonable, the prepared copper alloy has good processing performance and casting performance, and meanwhile, the alloy has the characteristics of high strength, good conductivity, excellent elasticity, strong high-temperature softening resistance and the like, can meet the requirements of the fields of electronic information, aerospace, transportation and the like, and has wide application prospects.

Description

High-strength and high-conductivity magnetic-compatibility copper alloy and preparation method of strip thereof
Technical Field
The invention belongs to the technical field of copper alloy materials and processes, and particularly relates to a high-strength and high-conductivity magnetic-compatibility copper alloy and a preparation method of a strip thereof.
Background
Copper alloys (copper alloys) are alloys made of pure copper as a matrix with one or several other elements added. The high-strength and high-conductivity copper alloy material is a structural functional material with excellent comprehensive physical properties and mechanical properties, has good mechanical and physical properties, and is widely applied to the industrial fields of electric power, electronics, machinery and the like. At present, many researches on high-strength and high-conductivity copper alloy materials are carried out, but researches on high-strength and high-conductivity magnetic compatible copper alloys are rare, and compared with common copper alloys, the high-strength and high-conductivity magnetic compatible copper alloys have excellent performances such as high anti-magnetic shielding, high conductivity, high strength and high elasticity, high weldability and the like, are new-generation high-end copper alloy materials meeting the requirements of the fields such as electronic information, aerospace, transportation and the like, have wide application fields and prospects for replacing old products, and have huge market using potential.
According to inspection, the Chinese patent with the prior patent number of 201811144609.0, namely the invention patent of a high-strength high-conductivity heat-resistant Cu-Fe-Y-Mg alloy material with electromagnetic wave shielding performance and a preparation method thereof, wherein the copper alloy comprises Cu, Fe, Mg and Y elements; and the mass percent of Fe is more than or equal to 5% and less than that of Cu, and the Fe is uniformly distributed in the alloy material. The copper alloy uses a large amount of cheap iron elements in component design, and because copper and iron are immiscible in a molten state, in the smelting process, the starting alloy mainly contains copper, a small amount of iron is added for smelting, after the copper is smelted, the Cu-Fe intermediate alloy is added in an intermediate alloy mode, and then the alloy elements yttrium and magnesium are jointly added in the smelting process to play a role of a modifier and promote the uniform distribution of an iron phase in a copper matrix in a solidification state. The copper alloy has electromagnetic wave shielding performance and high-strength high-conductivity heat resistance, but does not have good elasticity and high-temperature softening resistance, and needs further improvement.
Disclosure of Invention
The first technical problem to be solved by the invention is to provide a copper alloy which has scientific and reasonable component proportion, high alloy strength, high conductivity, magnetic compatibility and good electromagnetic shielding property, elasticity and high temperature softening resistance.
The second technical problem to be solved by the invention is to provide a preparation method of a high-strength and high-conductivity magnetic-compatibility copper alloy strip with a reasonable process, and the prepared copper alloy has the characteristics of good processing performance and casting performance, high alloy strength, good conductivity, excellent elasticity, strong high-temperature softening resistance and the like
The technical scheme adopted by the invention for solving the first technical problem is as follows: a high-strength and high-conductivity magnetic compatible copper alloy is characterized in that: the copper alloy comprises the following components in percentage by weight: fe: 5-6%, Ni: 0.01-2%, Si: 0.01-0.5%, Co: 0 to 0.1%, Nb: 0.007-0.012%, C: 0.01 to 0.1% by weight, and the balance copper and inevitable trace impurities.
Preferably, the copper alloy consists of the following components in percentage by weight: fe: 5.5%, Ni: 1.3%, Si: 0.3%, Co: 0.05%, Nb: 0.009%, C: 0.03 percent, and the balance of copper and inevitable trace impurities.
The technical scheme adopted by the invention for solving the second technical problem is as follows: a preparation method of a high-strength and high-conductivity magnetic-compatibility copper alloy strip is characterized by comprising the following steps: the method comprises the following steps:
1) material preparation and smelting: weighing the materials according to the component proportion of the copper alloy strip, adding Cu, Ni and Si into a smelting furnace, heating to melt, adding covering agent glass for covering after the copper liquid is melted, heating to 1400-1450 ℃, and slowly adding pure iron sheets with the thickness of 1.5-3 mm, the width of 20-50 mm and the length of 50-200 mm according to the alloy proportion; after the pure iron sheets are completely melted in the copper liquid, raising the temperature of the copper liquid to 1500-1550 ℃, adding a copper-niobium powder intermediate alloy wrapped by a copper pipe, preserving the heat for 20-30 minutes, then adding pure cobalt powder wrapped by the copper pipe, and preserving the heat for 15-30 minutes; then reducing the temperature to 1300-1350 ℃, preserving the heat for 1-2 h, introducing nitrogen with the pressure of 0.05-0.2 Mpa into a refining degassing stirrer, bringing 0.01-0.1% of powder spraying graphite into a rotary table of the refining degassing stirrer from a powder storage tank of the refining degassing stirrer, stirring and stirring copper liquid through the rotary table to uniformly distribute graphite powder and nitrogen into the copper liquid, wherein the rotating speed of a rotor is 300-350 r/min, and the degassing time is 4-6 min; adding 0.01-0.1% of carbon powder, keeping the temperature for 30 minutes, controlling the temperature to 1350-1400 ℃, fishing slag, and adding covering agents of cryolite and sodium carbonate for covering;
2) semi-continuous casting: controlling the temperature of the copper liquid at 1350-1450 ℃, pouring the smelting furnace, enabling the copper liquid to slowly flow into the chute and store a certain amount of copper liquid, then opening cooling water, controlling the water pressure to be about 30-70 Kpa, then rotating the stopper rod, starting a tractor when the height of the copper liquid in the crystallizer reaches two thirds of the height of the crystallizer, starting casting at 60-70 mm/min, starting vibration, wherein the frequency of a vibrator is 40-70 times/min, and the amplitude is 3-6 mm; then gradually increasing the casting speed and the cooling water strength until entering a speed stabilizing stage, wherein the casting speed of the speed stabilizing stage is controlled to be 90-130mm/min, and the water pressure is controlled to be 70-170 Kpa; adding a small amount of powdery covering agent cryolite, anhydrous borax and sodium carbonate into the crystallizer, and uniformly spraying the covering agent cryolite, anhydrous borax and sodium carbonate on the copper liquid surface;
3) hot rolling + on-line solid solution: heating the cast ingot at 950-980 ℃ for 1-1.5 h, keeping the temperature for hot rolling at 920-950 ℃, keeping the temperature for final rolling at more than 680 ℃, carrying out online spray cooling after final rolling, wherein the thickness of the hot rolled product is 9-11 mm, and the bandwidth is 435 +/-5 mm;
4) milling, rough rolling and trimming;
5) step aging: the temperature of the first stage aging is 500-550 ℃, the temperature is kept for 30min, the temperature of the second stage aging is 370-420 ℃, the temperature is kept for 6H, and the protective gas is full H2An atmosphere;
6) cleaning and then finish rolling;
7) and (3) stress relief annealing of a finished product: annealing at 170-200 ℃, and keeping the temperature for 5-8 h;
8) and cleaning, and then slitting and packaging the finished product.
As an improvement, the copper alloy strip in the step 1) has the following component proportion: fe: 5-6%, Ni: 0.01-2%, Si: 0.01-0.5%, Co: 0 to 0.1%, Nb: 0.007-0.012%, C: 0.01 to 0.1 percent of copper and inevitable trace impurities in percentage by mass.
Preferably, the copper alloy strip comprises the following components in percentage by weight: fe: 5.5%, Ni: 1.3%, Si: 0.3%, Co: 0.05%, Nb: 0.009%, C: 0.03 percent, and the balance of copper and inevitable trace impurities, wherein the percentages are mass percentages.
Preferably, the copper-niobium powder intermediate alloy wrapped by the copper pipe is added in the step 1), namely the copper-niobium alloy contains 4-6% of niobium, the alloy ingot is prepared by stirring, pressing, reducing and sintering copper powder and Nb powder into a powder alloy sheet, wherein the granularity of the Nb powder in the preparation process is less than or equal to 20 microns; the particle size of the cobalt powder added with pure cobalt powder wrapped by the copper pipe is 1-3 mm, and the weight ratio of covering agent cryolite and carbonic acid is 1: 1.
As an improvement, the semi-continuous casting crystallizer for semi-continuous casting in the step 2) adopts a special combined set of crystallizer, namely, the inner wall of the crystallizer adopts the materials of boron nitride and aluminum nitride, so that the problem that the graphite inner sleeve is corroded by the reaction of the graphite material adopted by the inner sleeve and Fe in the copper liquid for casting the alloy, and the surface of a semi-continuous casting blank is pulled to crack is solved; during the whole semi-continuous casting process, the stopper rod is adjusted to control the flow of copper liquid, so as to keep the liquid level in the crystallizer stable and maintain the liquid level height at about 10-20mm at the upper opening of the crystallizer; the weight ratio of the covering agent cryolite, the anhydrous borax and the sodium carbonate is 1:1: 1.
The surface milling in the step 4) is improved, wherein the surface milling amount is 0.6-0.8 mm on a single surface, and the thickness is 8-10 mm after surface milling; rough rolling means rolling thickness of 1.0 +/-0.015 mm; the trimming means that the single edge is sheared to be 10-15 mm, and the band width after shearing is 410 +/-0.5 mm.
Further, the step aging in the step 5) comprises the following specific steps: firstly, raising the temperature of a furnace to 500-550 ℃ according to the temperature rise rate of 120 ℃/h, preserving the temperature for 30min, and dissolving Ni and Si in an alloy matrix in a solid manner by using Ni2Rapidly precipitating a second Si strengthening phase; and then reducing the furnace temperature to 370-420 ℃ according to the cooling rate of 200 ℃/1h, preserving the temperature for 6h, and precipitating a large amount of solid-dissolved Fe and Co in the alloy matrix.
Finally, the specific cleaning process of the step 6) and the step 8) comprises the following steps: the degreasing agent adopts a p3 reagent (JQ-1 type metal cleaning agent) water solution, the pH range is 10-13, the solution temperature is 70-80 ℃, the pickling is carried out, the sulfuric acid concentration is 100-130 g/l, the temperature is less than or equal to 40 ℃, and Cu in acid liquor is adopted2+Less than or equal to 1.2g/l, adopting CC-2002/high-efficiency environment-friendly passivator for passivation, wherein the concentration of the solution is 0.07-0.12%, and cleaning and drying at the temperature of 80-100 ℃ in an oven; and 6) after finish rolling, the thickness is 0.2 +/-0.005 mm.
Nb, niobium is added into copper to refine grains and further improve the high temperature softening resistance, wear resistance and elasticity of the alloy, but when the content exceeds 0.02%, Nb is easy to form a coarse Nb-rich phase in the alloy, and the mechanical property of the alloy is deteriorated, so that the addition amount of Nb is controlled within 0.01% rather.
Co: a small amount of cobalt can delay the decomposition of solid solution, reduce the desolvation speed of a crystal boundary, inhibit the reaction of the crystal boundary and obviously delay aging softening, thereby further improving the mechanical property of the alloy, but the cobalt can reduce the conductivity of the alloy, so the component is properly controlled within 0.05 percent.
Compared with the prior art, the invention has the advantages that: the formula is scientific and reasonable, niobium and cobalt are added, the niobium is added into copper to refine grains, the high temperature softening performance, the wear resistance and the elasticity of the alloy are further improved, a small amount of cobalt can delay the decomposition of solid solution, reduce the desolventizing speed of a grain boundary, inhibit the reaction of the grain boundary and obviously delay aging softening, so that the mechanical property of the alloy is further improved. The preparation process is reasonable, and the prepared copper alloy has the characteristics of good processability and castability, high alloy strength, good conductivity, excellent elasticity, strong high-temperature softening resistance and the like, can meet the requirements of the fields of electronic information, aerospace, transportation and the like, and has wide application prospect.
Drawings
Figure 1 is a cross-sectional metallographic picture of the finished strip of example 4 provided by the invention.
Detailed Description
The invention is described in further detail below with reference to the accompanying examples.
Table 1 shows the composition ratios of the copper alloy strip of four examples of the invention:
alloy chemical composition (wt%) of the embodiment of the invention
Material numbering Fe Ni Co Nb C Si Cu
Example 1 5.9 0.9 0.06 0.007 0.012 0.2 Balance of
Example 2 5.7 1.5 0.03 0.008 0.02 0.38 Balance of
Example 3 5.2 1.8 0.08 0.01 0.035 0.42 Balance of
Preferred embodiment 4 5.5 1.3 0.05 0.009 0.03 0.3 Balance of
Example 1
1) Material preparation and smelting: weighing the components according to the component proportion of the copper alloy strip, adding Cu, Ni and Si into a smelting furnace, heating to melt, and adding covering agent glass for covering after the copper liquid is melted. And then, raising the temperature to 1400-1450 ℃, and slowly adding pure iron sheets with the thickness of 1.5-3 mm, the width of 20-50 mm and the length of 50-200 mm according to the alloy proportion. After the pure iron sheets are completely melted in the copper liquid, the temperature of the copper liquid is raised to 1520 ℃, the copper niobium powder intermediate alloy wrapped by the copper pipe is added, the temperature is kept for 20 minutes, then the pure cobalt powder wrapped by the copper pipe is added, and the temperature is kept for 25 minutes. And then, reducing the temperature to 1300-1350 ℃, preserving the heat for 1-2 h, introducing nitrogen with the pressure of 0.05-0.2 Mpa into a refining degassing stirrer, bringing 0.012% of powder spraying graphite into a rotary disc of the refining degassing stirrer from a powder storage tank of the refining degassing stirrer, stirring and stirring copper liquid by the rotary disc to uniformly distribute graphite powder and nitrogen into the copper liquid, wherein the rotating speed of a rotor is 300-350 r/min, and the degassing time is 5 minutes. The process can achieve the effects of refining, degassing, homogenizing components and adding trace C elements. Adding 0.012 percent of carbon powder, keeping the temperature for 30 minutes, controlling the temperature to 1350-1400 ℃, fishing slag, and adding covering agent cryolite and sodium carbonate (the weight ratio is 1:1) for covering.
2) Semi-continuous casting: and controlling the temperature of the copper liquid to 1350-1450 ℃, pouring the smelting furnace, and enabling the copper liquid to slowly flow into the chute and store a certain amount of copper liquid. Then, opening cooling water, controlling the water pressure to be about 50Kpa, rotating the stopper rod, starting a tractor when the height of copper liquid in the crystallizer reaches about two thirds of that of the crystallizer, starting drawing and casting at 60mm/min, starting vibration, controlling the frequency of a vibrator to be 45 times/min and the amplitude to be 5mm, then gradually increasing the drawing and casting speed and increasing the strength of the cooling water until a speed stabilizing stage is started, controlling the casting speed at 90mm/min and controlling the water pressure at 120Kpa in the speed stabilizing stage; in the whole process, the stopper rod is adjusted to control the flow of copper liquid, the liquid level in the crystallizer is kept stable as much as possible, the liquid level height is preferably maintained at about 10-20mm of the upper opening of the crystallizer, and a small amount of powdery covering agent cryolite, anhydrous borax and sodium carbonate (the weight ratio of the covering agent cryolite to the anhydrous borax to the sodium carbonate is 1:1:1) are added into the crystallizer and uniformly sprayed on the copper liquid level, so that a thin molten covering agent layer covers the liquid level in the crystallizer; the semi-continuous casting crystallizer adopts a special combined set, namely the inner wall of the crystallizer adopts the materials of boron nitride and aluminum nitride, so that the problem that the surface of a semi-continuous casting blank is pulled to crack due to the fact that the graphite inner sleeve is corroded by the reaction of the graphite material and Fe in the copper liquid for casting the alloy is solved.
3) Hot rolling + on-line solid solution: the ingot is heated at 960 ℃, the heat preservation time is 1.5h, the hot rolling start temperature is 930 ℃, the finish rolling temperature is 690 ℃, the online spray cooling is carried out after the finish rolling, the thickness after the hot rolling is 10 +/-0.1 mm, and the bandwidth is 435 +/-5 mm.
4) Milling a surface: the milling amount of the single surface is 0.7mm, and the thickness after milling is 8.6 mm;
6) rough rolling: the rolling thickness is 1.0 +/-0.015 mm;
7) trimming: the unilateral shearing is 10-15 mm, and the band width after shearing is 410 +/-0.5 mm;
8) step aging: the first stage aging temperature is 550 ℃, and the temperature is kept for 30 min. The secondary aging temperature is 370 ℃, and the temperature is kept for 6 h. The protective gas is full H2An atmosphere. Firstly, raising the temperature of the furnace to 550 ℃ according to the heating rate of 120 ℃/h, preserving the temperature for 30min, and dissolving Ni and Si in the alloy matrix in a solid manner by using Ni2The Si second strengthening phase is rapidly precipitated and dispersed in the structure, so that the solid solution aging strengthening effect is achieved, and the strength, elasticity, conductivity, high temperature softening resistance and the like of the alloy are improved. Secondly, the furnace temperature is reduced to 370 ℃ according to the cooling rate of 200 ℃/1h, the temperature is kept for 6h, a large amount of solid-dissolved Fe and Co in the alloy matrix are precipitated, the electromagnetic property, the electric conductivity, the wear resistance and the like of the alloy are improved, and meanwhile, the matrix is further promoted to be inSolid-dissolved Ni and Si, with Ni2And Si is precipitated in a second strengthening way, so that the comprehensive performance of the alloy is improved. The annealing furnace adopts full H2And (5) gas reduction protection.
9) Cleaning: the degreasing agent is a p3 reagent (JQ-1 type metal cleaning agent) water solution, the PH range is 10-13, and the solution temperature is 70-80 ℃. Acid washing, wherein the concentration of sulfuric acid is 100-130 g/l, the temperature is less than or equal to 40 ℃, and Cu is contained in acid liquor2+Less than or equal to 1.2g/l, adopting CC-2002/high-efficiency environment-friendly passivator for passivation, wherein the concentration of the solution is 0.07-0.12%, and cleaning and drying the mixture at the temperature of 80-100 ℃ in an oven.
10) Finish rolling: the thickness after finish rolling is 0.2 +/-0.005 mm.
11) Stress relief annealing of the finished product; the annealing temperature is 200 ℃, and the heat preservation is carried out for 5 hours.
12) Cleaning: the degreasing agent is a p3 reagent (JQ-1 type metal cleaning agent) water solution, the PH range is 10-13, and the solution temperature is 70-80 ℃. Acid washing, wherein the concentration of sulfuric acid is 80-100 g/l, the temperature is less than or equal to 40 ℃, and Cu is contained in acid liquor2+Less than or equal to 1.1g/l, adopting CC-2002/high-efficiency environment-friendly passivator for passivation, wherein the concentration of the solution is 0.07-0.12%, and cleaning and drying the mixture at the temperature of 80-100 ℃ in an oven.
13) And (5) splitting and packaging the finished product.
Example 2
1) Material preparation and smelting: weighing the materials according to the component proportion of the copper alloy strip, adding Cu, Ni and Si into a smelting furnace, heating to melt, adding covering agent glass for covering after the copper liquid is melted, then heating to 1400-1450 ℃, and slowly adding pure iron sheets with the thickness of 1.5-3 mm, the width of 20-50 mm and the length of 50-200 mm according to the alloy proportion. After the pure iron sheet is completely melted in the copper liquid, the temperature of the copper liquid is raised to 1550 ℃, the copper niobium powder intermediate alloy wrapped by the copper pipe is added, and the temperature is kept for 20 minutes, then pure cobalt powder wrapped by a copper pipe is added, the temperature is kept for 30 minutes, then reducing the temperature to 1300-1350 ℃, preserving the heat for 1-2 h, then adopting a refining degassing stirrer, introducing nitrogen with the pressure of 0.05-0.2 Mpa, bringing 0.02 percent of powder spraying graphite into a rotary table of the refining degassing stirrer from a powder storage tank of the refining degassing stirrer, and then stirring and stirring the copper liquid by a turntable to uniformly distribute graphite powder and nitrogen in the copper liquid, wherein the rotation speed of a rotor is 300-350 r/min, the degassing time is 5 minutes, the effects of refining, degassing, homogenizing components and adding trace C element are achieved in the process, 0.02% of carbon powder is added, the temperature is controlled to 1350-1400 ℃ after heat preservation is carried out for 30 minutes, slag is fished, and covering agent cryolite and sodium carbonate (the weight ratio is 1:1) are added for covering.
2) Semi-continuous casting: and controlling the temperature of the copper liquid to 1350-1450 ℃, pouring the smelting furnace, and enabling the copper liquid to slowly flow into the chute and store a certain amount of copper liquid. Then, opening cooling water, controlling the water pressure to be about 70Kpa, rotating the stopper rod, starting a tractor when the height of the copper liquid in the crystallizer reaches about two thirds of the height of the crystallizer, starting casting at 60mm/min, starting vibration, controlling the frequency of a vibrator for 50 times/min, controlling the amplitude to be 4mm, then gradually increasing the casting speed and increasing the strength of the cooling water until the crystallizer enters a speed stabilizing stage, controlling the casting speed at 120mm/min and the water pressure at 130Kpa, and in the whole process, paying attention to the adjustment of the stopper rod to control the flow of the copper liquid, keeping the liquid level in the crystallizer as stable as possible, and preferably maintaining the liquid level at about 10-20mm of the upper opening of the crystallizer; and adding a small amount of powdery covering agent cryolite, anhydrous borax and sodium carbonate (the weight ratio of the covering agent cryolite to the anhydrous borax to the sodium carbonate is 1:1:1) into the crystallizer, and uniformly spraying the covering agent cryolite, the anhydrous borax and the sodium carbonate on the copper liquid surface to cover a thin molten covering agent layer on the liquid surface in the crystallizer. The semi-continuous casting crystallizer adopts a special combined set, namely the inner wall of the crystallizer adopts the materials of boron nitride and aluminum nitride, so that the problem that the surface of a semi-continuous casting blank is pulled to crack due to the fact that the graphite inner sleeve is corroded by the reaction of the graphite material and Fe in the copper liquid for casting the alloy is solved.
3) Hot rolling + on-line solid solution: the ingot casting heating temperature is 970 ℃, the heat preservation time is 1.5h, the hot rolling starting temperature is 940 ℃, the finish rolling temperature is 725 ℃, the online spray cooling is carried out after the finish rolling, the thickness after the hot rolling is 10.3 +/-0.1 mm, and the bandwidth is 435 +/-5 mm.
4) Milling a surface: the milling amount of the single surface is 0.7mm, and the thickness after milling is 9.9 mm;
6) rough rolling; the rolling thickness is 1.0 +/-0.015 mm;
7) trimming; the unilateral shearing is 10-15 mm, and the band width after shearing is 410 +/-0.5 mm;
8) step aging; the first-stage aging temperature is 500 ℃,and preserving the heat for 30 min. The temperature of the second stage aging is 420 ℃, and the temperature is kept for 6 h. The protective gas is full H2An atmosphere. Firstly, raising the temperature of the furnace to 500 ℃ according to the heating rate of 120 ℃/h, preserving the temperature for 30min, and dissolving Ni and Si in the alloy matrix in a solid manner by using Ni2The Si second strengthening phase is rapidly precipitated and dispersed in the structure, so that the solid solution aging strengthening effect is achieved, and the strength, elasticity, conductivity, high temperature softening resistance and the like of the alloy are improved. Secondly, the furnace temperature is reduced to 420 ℃ according to the cooling rate of 200 ℃/1h, the temperature is kept for 6h, a large amount of solid-dissolved Fe and Co in the alloy matrix are precipitated, the electromagnetic property, the electric conductivity, the wear resistance and the like of the alloy are improved, and meanwhile, the solid-dissolved Ni and Si in the matrix are further promoted, and Ni is used as Ni2And Si is precipitated in a second strengthening way, so that the comprehensive performance of the alloy is improved. The annealing furnace adopts full H2And (5) gas reduction protection.
9) Cleaning; the degreasing agent is a p3 reagent (JQ-1 type metal cleaning agent) water solution, the PH range is 10-13, and the solution temperature is 70-80 ℃. Acid washing, wherein the concentration of sulfuric acid is 100-130 g/l, the temperature is less than or equal to 40 ℃, and Cu is contained in acid liquor2+Less than or equal to 1.2g/l, adopting CC-2002/high-efficiency environment-friendly passivator for passivation, wherein the concentration of the solution is 0.07-0.12%, and cleaning and drying the mixture at the temperature of 80-100 ℃ in an oven.
10) Finish rolling: the thickness after finish rolling is 0.2 +/-0.005 mm.
11) Stress relief annealing of the finished product; the annealing temperature is 200 ℃, and the heat preservation is carried out for 5 hours.
12) Cleaning; the degreasing agent is a p3 reagent (JQ-1 type metal cleaning agent) water solution, the PH range is 10-13, and the solution temperature is 70-80 ℃. Acid washing, wherein the concentration of sulfuric acid is 80-100 g/l, the temperature is less than or equal to 40 ℃, and Cu is contained in acid liquor2+Less than or equal to 1.1g/l, adopting CC-2002/high-efficiency environment-friendly passivator for passivation, wherein the concentration of the solution is 0.07-0.12%, and cleaning and drying the mixture at the temperature of 80-100 ℃ in an oven.
13) And (5) splitting and packaging the finished product.
Example 3
1) Material preparation and smelting: weighing the materials according to the component proportion of the copper alloy strip, adding Cu, Ni and Si into a smelting furnace, heating to melt, and adding covering agent glass for covering after the copper liquid is melted; and then, raising the temperature to 1400-1450 ℃, and slowly adding pure iron sheets with the thickness of 1.5-3 mm, the width of 20-50 mm and the length of 50-200 mm according to the alloy proportion. After the pure iron sheets are completely melted in the copper liquid, the temperature of the copper liquid is raised to 1540 ℃, the copper niobium powder intermediate alloy wrapped by the copper pipe is added, the temperature is kept for 30 minutes, then the pure cobalt powder wrapped by the copper pipe is added, and the temperature is kept for 15 minutes. And then, reducing the temperature to 1300-1350 ℃, preserving the temperature for 1-2 h, introducing nitrogen with the pressure of 0.05-0.2 Mpa into a refining degassing stirrer, bringing 0.035% of powder spraying graphite into a rotary table of the refining degassing stirrer from a powder storage tank of the refining degassing stirrer, stirring and stirring copper liquid through the rotary table to uniformly distribute graphite powder and nitrogen into the copper liquid, wherein the rotating speed of a rotor is 300-350 r/min, and the degassing time is 5 minutes. The effects of refining, degassing, homogenizing components and adding trace C elements are achieved in the process; adding 0.035% carbon powder, keeping the temperature for 30 minutes, controlling the temperature at 1350-1400 ℃, dragging slag, and adding covering agent cryolite and sodium carbonate (weight ratio 1:1) for covering.
2) Semi-continuous casting: controlling the temperature of the copper liquid to 1350-1450 ℃, pouring the smelting furnace, and enabling the copper liquid to slowly flow into the chute and store a certain amount of copper liquid; and then, opening cooling water, controlling the water pressure to be about 60Kpa, rotating the stopper rod, starting a tractor when the height of the copper liquid in the crystallizer reaches about two thirds of the height of the crystallizer, starting the casting at 60mm/min, starting vibration, and controlling the frequency of a vibrator to be 50 times/min and the amplitude to be 6 mm. Then gradually increasing the casting speed and the cooling water strength until entering a speed stabilizing stage, controlling the casting speed at 110mm/min and controlling the water pressure at 150Kpa in the speed stabilizing stage; in the whole process, the stopper rod is adjusted to control the flow of the copper liquid, the liquid level in the crystallizer is kept stable as much as possible, and the liquid level height is preferably kept about 10-20mm at the upper opening of the crystallizer; adding a small amount of powdery covering agent cryolite, anhydrous borax and sodium carbonate (the weight ratio of the covering agent cryolite to the anhydrous borax to the sodium carbonate is 1:1:1) into the crystallizer, and uniformly spraying the covering agent cryolite, the anhydrous borax and the sodium carbonate on the copper liquid surface to cover a thin molten covering agent layer on the liquid surface in the crystallizer; the semi-continuous casting crystallizer adopts a special combined set, namely the inner wall of the crystallizer adopts the materials of boron nitride and aluminum nitride, so that the problem that the surface of a semi-continuous casting blank is pulled to crack due to the fact that the graphite inner sleeve is corroded by the reaction of the graphite material and Fe in the copper liquid for casting the alloy is solved.
3) Hot rolling + on-line solid solution: heating the ingot at 970 ℃, keeping the temperature for 1h, starting the hot rolling at 940 ℃, finishing the ingot at 710 ℃, carrying out on-line spray cooling after finishing the ingot, and carrying out hot rolling to obtain the ingot with the thickness of 10.5 +/-0.1 mm and the bandwidth of 435 +/-5 mm.
4) Milling a surface: the milling amount of the single surface is 0.75mm, and the thickness after milling is 9 mm;
6) rough rolling: the rolling thickness is 1.0 +/-0.015 mm;
7) trimming: the unilateral shearing is 10-15 mm, and the band width after shearing is 410 +/-0.5 mm;
8) step aging; the first stage aging temperature is 530 ℃, and the temperature is kept for 30 min. The secondary aging temperature is 400 ℃, and the heat preservation is carried out for 6 hours. The protective gas is full H2An atmosphere. Firstly, raising the temperature of the furnace to 530 ℃ according to the heating rate of 120 ℃/h, preserving the temperature for 30min, and dissolving Ni and Si in the alloy matrix in a solid manner by using Ni2The Si second strengthening phase is rapidly precipitated and dispersed in the structure, so that the solid solution aging strengthening effect is achieved, and the strength, elasticity, conductivity, high temperature softening resistance and the like of the alloy are improved. Secondly, the furnace temperature is reduced to 400 ℃ according to the cooling rate of 200 ℃/1h, the temperature is kept for 6h, a large amount of solid-dissolved Fe and Co in the alloy matrix are precipitated, the electromagnetic property, the electric conductivity, the wear resistance and the like of the alloy are improved, and meanwhile, the solid-dissolved Ni and Si in the matrix are further promoted, and Ni is used as Ni2And Si is precipitated in a second strengthening way, so that the comprehensive performance of the alloy is improved. The annealing furnace adopts full H2And (5) gas reduction protection.
9) Cleaning; the degreasing agent is a p3 reagent (JQ-1 type metal cleaning agent) water solution, the PH range is 10-13, and the solution temperature is 70-80 ℃. Acid washing, wherein the concentration of sulfuric acid is 100-130 g/l, the temperature is less than or equal to 40 ℃, and Cu is contained in acid liquor2+Less than or equal to 1.2g/l, adopting CC-2002/high-efficiency environment-friendly passivator for passivation, wherein the concentration of the solution is 0.07-0.12%, and cleaning and drying the mixture at the temperature of 80-100 ℃ in an oven.
10) Finish rolling: the thickness after finish rolling is 0.2 +/-0.005 mm.
11) Stress relief annealing of the finished product; the annealing temperature is 175 ℃, and the temperature is kept for 7 h.
12) Cleaning: the degreasing agent is a p3 reagent (JQ-1 type metal cleaning agent) water solution, the PH range is 10-13, and the solution temperature is 70-80 ℃. Acid washing, the concentration of sulfuric acid is 80-100 g/l, and the temperature isCu in acid liquor at 40 deg.C or below2+Less than or equal to 1.1g/l, adopting CC-2002/high-efficiency environment-friendly passivator for passivation, wherein the concentration of the solution is 0.07-0.12%, and cleaning and drying the mixture at the temperature of 80-100 ℃ in an oven.
13) And (5) splitting and packaging the finished product.
Preferred embodiment 4
1) Material preparation and smelting: weighing the materials according to the component proportion of the copper alloy strip, adding Cu, Ni and Si into a smelting furnace, heating to melt, and adding covering agent glass for covering after the copper liquid is melted; and then, raising the temperature to 1400-1450 ℃, and slowly adding pure iron sheets with the thickness of 1.5-3 mm, the width of 20-50 mm and the length of 50-200 mm according to the alloy proportion. After the pure iron sheet is completely melted in the copper liquid, raising the temperature of the copper liquid to 1550 ℃, adding a copper-niobium powder intermediate alloy wrapped by a copper pipe, and preserving the heat for 20 minutes, wherein the copper-niobium powder intermediate alloy wrapped by the copper pipe is added, namely the copper-niobium alloy contains 4-6% of niobium, and an alloy ingot is stirred, pressed, reduced and sintered into a powder alloy sheet by adopting copper powder and Nb powder; wherein the granularity of the Nb powder in the preparation process is less than or equal to 20 mu m; then adding pure cobalt powder wrapped by a copper pipe, wherein the particle size of the cobalt powder is 1-3 mm, and keeping the temperature for 20 minutes; then reducing the temperature to 1300-1350 ℃, preserving the heat for 1-2 h, introducing nitrogen with the pressure of 0.05-0.2 Mpa into a refining degassing stirrer, carrying 0.03% of powder spraying graphite into a rotary table of the refining degassing stirrer from a powder storage tank of the refining degassing stirrer, stirring and stirring copper liquid through the rotary table to uniformly distribute graphite powder and nitrogen into the copper liquid, wherein the rotating speed of a rotor is 300-350 r/min, and the degassing time is 5 min; the process can achieve the effects of refining, degassing, homogenizing components and adding trace C elements. Adding 0.03% carbon powder, keeping the temperature for 30 minutes, controlling the temperature to 1350-1400 ℃, fishing slag, and adding covering agent cryolite and sodium carbonate (weight ratio is 1:1) for covering.
2) Semi-continuous casting: and controlling the temperature of the copper liquid to 1350-1450 ℃, pouring the smelting furnace, and enabling the copper liquid to slowly flow into the chute and store a certain amount of copper liquid. Then, opening cooling water, controlling the water pressure to be about 60Kpa, rotating the stopper rod, starting a tractor when the height of the copper liquid in the crystallizer reaches about two thirds of the height of the crystallizer, starting the casting at 65mm/min, starting vibration, and controlling the frequency of a vibrator to be 55 times/min and the amplitude to be 5 mm; then gradually increasing the casting speed and the cooling water strength until entering a speed stabilizing stage, controlling the casting speed at 115mm/min and the water pressure at 120Kpa in the speed stabilizing stage; in the whole process, the stopper rod is adjusted to control the flow of the copper liquid, the liquid level in the crystallizer is kept stable as much as possible, and the liquid level height is preferably kept about 10-20mm at the upper opening of the crystallizer. Adding a small amount of powdery covering agent cryolite, anhydrous borax and sodium carbonate (the weight ratio of the covering agent cryolite to the anhydrous borax to the sodium carbonate is 1:1:1) into the crystallizer, and uniformly spraying the covering agent cryolite, the anhydrous borax and the sodium carbonate on the copper liquid surface to cover a thin molten covering agent layer on the liquid surface in the crystallizer; the semi-continuous casting crystallizer adopts a special combined set, namely the inner wall of the crystallizer adopts the materials of boron nitride and aluminum nitride, so that the problem that the surface of a semi-continuous casting blank is pulled to crack due to the fact that the graphite inner sleeve is corroded by the reaction of the graphite material and Fe in the copper liquid for casting the alloy is solved.
3) Hot rolling + on-line solid solution: the ingot is heated at 960 ℃, the heat preservation time is 1.5h, the hot rolling start temperature is 930 ℃, the finish rolling temperature is 725 ℃, the online spray cooling is carried out after the finish rolling, the thickness after the hot rolling is 10.5 +/-0.1 mm, and the bandwidth is 435 +/-5 mm.
4) Milling a surface: the milling amount of the single surface is 0.75mm, and the thickness after milling is 9 mm;
6) rough rolling: the rolling thickness is 1.0 +/-0.015 mm;
7) trimming: the unilateral shearing is 10-15 mm, and the band width after shearing is 410 +/-0.5 mm;
8) step aging; the first stage aging temperature is 510 ℃, and the temperature is kept for 30 min. The secondary aging temperature is 380 ℃, and the temperature is kept for 6 h. The protective gas is full H2An atmosphere. Firstly, the furnace temperature is increased to 510 ℃ according to the heating rate of 120 ℃/h, the temperature is kept for 30min, and Ni and Si which are dissolved in an alloy matrix are mixed with Ni2The Si second strengthening phase is rapidly precipitated and dispersed in the structure, so that the solid solution aging strengthening effect is achieved, and the strength, elasticity, conductivity, high temperature softening resistance and the like of the alloy are improved. Secondly, the furnace temperature is reduced to 380 ℃ according to the cooling rate of 200 ℃/1h, the temperature is kept for 6h, a large amount of solid-dissolved Fe and Co in the alloy matrix are precipitated, the electromagnetic property, the electric conductivity, the wear resistance and the like of the alloy are improved, and meanwhile, the matrix is further promoted to be inSolid-dissolved Ni and Si, with Ni2And Si is precipitated in a second strengthening way, so that the comprehensive performance of the alloy is improved. The annealing furnace adopts full H2And (5) gas reduction protection.
9) Cleaning: the degreasing agent is a p3 reagent (JQ-1 type metal cleaning agent) water solution, the PH range is 10-13, and the solution temperature is 70-80 ℃. Acid washing, wherein the concentration of sulfuric acid is 100-130 g/l, the temperature is less than or equal to 40 ℃, and Cu is contained in acid liquor2+Less than or equal to 1.2g/l, adopting CC-2002/high-efficiency environment-friendly passivator for passivation, wherein the concentration of the solution is 0.07-0.12%, and cleaning and drying the mixture at the temperature of 80-100 ℃ in an oven.
10) Finish rolling: the thickness after finish rolling is 0.2 +/-0.005 mm.
11) And (3) stress relief annealing of a finished product: the annealing temperature is 170 ℃, and the heat preservation is carried out for 8 hours.
12) Cleaning; the degreasing agent is a p3 reagent (JQ-1 type metal cleaning agent) water solution, the PH range is 10-13, and the solution temperature is 70-80 ℃. Acid washing, wherein the concentration of sulfuric acid is 80-100 g/l, the temperature is less than or equal to 40 ℃, and Cu is contained in acid liquor2+Less than or equal to 1.1g/l, adopting CC-2002/high-efficiency environment-friendly passivator for passivation, wherein the concentration of the solution is 0.07-0.12%, and cleaning and drying the mixture at the temperature of 80-100 ℃ in an oven.
13) And (5) splitting and packaging the finished product.
Table 2 shows the results of the performance tests of the copper alloy wires prepared in the above four examples:
TABLE 2 product Performance parameters
Figure BDA0002187982510000111
FIG. 1 is a cross-sectional metallographic picture of a 0.2mm strip of the finished product of example 4, the product of example 4 having the best overall properties compared with the results of the performance tests of Table 2.

Claims (7)

1. A preparation method of a high-strength and high-conductivity magnetic-compatibility copper alloy strip is characterized by comprising the following steps: the method comprises the following steps:
1) material preparation and smelting: weighing the copper alloy strip according to the component proportion, adding Cu, Ni and Si into a smelting furnace, heating to melt, adding covering agent glass for covering after a copper liquid is melted, then heating to 1400-1450 ℃, and slowly adding pure iron sheets with the thickness of 1.5-3 mm, the width of 20-50 mm and the length of 50-200 mm according to the alloy proportion; after the pure iron sheets are completely melted in the copper liquid, raising the temperature of the copper liquid to 1500-1550 ℃, adding a copper-niobium powder intermediate alloy wrapped by a copper pipe, preserving the heat for 20-30 minutes, then adding pure cobalt powder wrapped by the copper pipe, and preserving the heat for 15-30 minutes; then reducing the temperature to 1300-1350 ℃, preserving the temperature for 1-2 h, introducing nitrogen with the pressure of 0.05-0.2 MPa into a refining degassing stirrer, bringing 0.01-0.1% of powder spraying graphite into a rotary table of the refining degassing stirrer from a powder storage tank of the refining degassing stirrer, then stirring copper liquid through rotation of the rotary table to uniformly distribute graphite powder and nitrogen into the copper liquid, wherein the rotation speed of a rotor is 300-350 r/min, and the degassing time is 4-6 min; adding 0.01-0.1% of carbon powder, keeping the temperature for 30 minutes, controlling the temperature to 1350-1400 ℃, fishing slag, and adding covering agents of cryolite and sodium carbonate for covering;
the copper alloy strip in the step 1) comprises the following components in percentage by weight: fe: 5-6%, Ni: 0.01-2%, Si: 0.01-0.5%, Co: 0.03-0.1%, Nb: 0.007-0.012%, C: 0.01-0.1 percent of copper and inevitable trace impurities in percentage by mass;
2) semi-continuous casting: controlling the temperature of the copper liquid at 1350-1450 ℃, pouring the smelting furnace, enabling the copper liquid to slowly flow into the chute and store a certain amount of copper liquid, then opening cooling water, controlling the water pressure at the moment to be 30-70 kPa, rotating the stopper rod, starting a tractor when the height of the copper liquid in the crystallizer reaches two thirds of the height of the crystallizer, starting casting at 60-70 mm/min, starting vibration, and enabling the frequency of a vibrator to be 40-70 times/min and the amplitude to be 3-6 mm; then gradually increasing the casting speed and the cooling water strength until entering a speed stabilizing stage, wherein the casting speed in the speed stabilizing stage is controlled to be 90-130mm/min, and the water pressure is controlled to be 70-170 kPa; adding a small amount of powdery covering agent cryolite, anhydrous borax and sodium carbonate into the crystallizer, and uniformly spraying the covering agent cryolite, anhydrous borax and sodium carbonate on the copper liquid surface;
3) hot rolling + on-line solid solution: heating the cast ingot at 950-980 ℃ for 1-1.5 h, starting hot rolling at 920-950 ℃, finishing rolling at more than 680 ℃, carrying out on-line spray cooling after finishing rolling, wherein the thickness of the hot rolled product is 9-11 mm, and the bandwidth is 435 +/-5 mm;
4) milling, rough rolling and trimming;
5) step aging: the temperature of the first stage aging is 500-550 ℃, the temperature is kept for 30min, the temperature of the second stage aging is 370-420 ℃, the temperature is kept for 6H, and the protective gas is full H2An atmosphere;
6) cleaning and then finish rolling;
7) and (3) stress relief annealing of a finished product: annealing at 170-200 ℃, and keeping the temperature for 5-8 h;
8) and cleaning, and then slitting and packaging the finished product.
2. The method of claim 1, wherein: the copper alloy strip comprises the following components in percentage by weight: fe: 5.5%, Ni: 1.3%, Si: 0.3%, Co: 0.05%, Nb: 0.009%, C: 0.03 percent, and the balance of copper and inevitable trace impurities, wherein the percentages are mass percentages.
3. The method of claim 1, wherein: the copper-niobium powder intermediate alloy wrapped by the copper pipe in the step 1) is added, namely the copper-niobium alloy contains 4-6% of niobium, the alloy ingot is prepared by stirring, pressing, reducing and sintering copper powder and Nb powder into a powder alloy sheet, wherein the granularity of the Nb powder in the preparation process is less than or equal to 20 microns; the particle size of the cobalt powder added with pure cobalt powder wrapped by a copper pipe is 1-3 mm, and the weight ratio of covering agent cryolite to sodium carbonate is 1: 1.
4. The method of claim 1, wherein: the semi-continuous casting crystallizer for the semi-continuous casting in the step 2) adopts a crystallizer with a combined sleeve, namely the inner wall of the crystallizer adopts the materials of boron nitride and aluminum nitride, the stopper rod is required to be adjusted in the whole semi-continuous casting process so as to control the flow of copper liquid, keep the liquid level in the crystallizer stable and maintain the liquid level height at the upper opening of the crystallizer by 10-20 mm; the weight ratio of the covering agent cryolite, the anhydrous borax and the sodium carbonate is 1:1: 1.
5. The method of claim 1, wherein: the surface milling in the step 4) is to mill the surface of a single surface by 0.6-0.8 mm, and the thickness of the milled surface is 8-10 mm; rough rolling means rolling thickness of 1.0 +/-0.015 mm; the trimming means that the single edge is sheared to be 10-15 mm, and the band width after shearing is 410 +/-0.5 mm.
6. The method of claim 1, wherein: the step aging in the step 5) comprises the following specific steps: firstly, raising the temperature of a furnace to 500-550 ℃ according to the temperature rise rate of 120 ℃/h, preserving the temperature for 30min, and dissolving Ni and Si in an alloy matrix in a solid manner by using Ni2Rapidly precipitating a second Si strengthening phase; and then reducing the furnace temperature to 370-420 ℃ according to the cooling rate of 200 ℃/1h, preserving the temperature for 6h, and precipitating a large amount of solid-dissolved Fe and Co in the alloy matrix.
7. The method of claim 1, wherein: the specific cleaning process of the step 6) and the step 8) comprises the following steps: the degreasing agent adopts JQ-1 type metal cleaner water solution, the pH range is 10-13, the solution temperature is 70-80 ℃, the pickling is carried out, the sulfuric acid concentration is 100-130 g/L, the temperature is less than or equal to 40 ℃, and Cu in the acid solution is2+Less than or equal to 1.2g/L, adopting a CC-2002 high-efficiency environment-friendly passivating agent for passivation, cleaning and drying, wherein the solution concentration is 0.07-0.12%, and the oven temperature is 80-100 ℃; and 6) after finish rolling, the thickness is 0.2 +/-0.005 mm.
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