CN113088755A - Copper wire with good conductivity and preparation method thereof - Google Patents
Copper wire with good conductivity and preparation method thereof Download PDFInfo
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- CN113088755A CN113088755A CN202110353865.6A CN202110353865A CN113088755A CN 113088755 A CN113088755 A CN 113088755A CN 202110353865 A CN202110353865 A CN 202110353865A CN 113088755 A CN113088755 A CN 113088755A
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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
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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
- C22C1/03—Making non-ferrous alloys by melting using master alloys
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B1/00—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors
- H01B1/02—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors mainly consisting of metals or alloys
- H01B1/026—Alloys based on copper
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B13/00—Apparatus or processes specially adapted for manufacturing conductors or cables
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Abstract
The invention discloses a copper wire with good conductivity and a preparation method thereof, copper and silver are compounded to prepare copper-based alloy, the conductivity of the material is increased, lanthanum is added in the compounding process, the lanthanum interacts with inevitable impurities in the copper and silver to form an indissolvable high-melting-point binary or multicomponent compound, the distortion is weakened, crystals become more compact and regular to reduce the resistivity of the alloy, and the Mg-Ca alloy, lead and lithium act together to further increase the density and simultaneously increase the mechanical property of the alloy, the lanthanum and lithium act to eliminate the hot brittleness of the lead, so that the mechanical property is not weakened while the resistivity is reduced, benzotriazole cooperates with the lanthanum and Mg-Ca alloy to increase the corrosion resistance of the material, and the material is more compact and the heat damage of the copper and the silver is reduced by the way of firstly compounding the copper and the silver to prepare the alloy and then crushing the alloy, the mechanical property of the material is increased.
Description
Technical Field
The invention relates to a copper wire with good conductivity and a production method thereof.
Background
In recent years, silver-copper alloy has high conductivity and is greatly concerned in the fields of conductive paste, conductive ink and conductive fine wiring, but the silver-copper alloy has obvious defects, poor mechanical property, poor corrosion resistance and easy yielding, so that the silver-copper alloy is not well developed in aerospace and high-temperature and high-humidity environments.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provide a copper wire with good conductivity and a preparation method thereof.
In order to solve the technical problems, the invention adopts the following technical scheme,
a copper wire with good conductivity comprises the following basic components in percentage by weight: 6 to 15 percent of Ag, 0.02 to 1 percent of Mg-Ca alloy, 0.02 to 0.045 percent of La, 1 to 3.3 percent of Le, 0.005 to 0.045 percent of Pb and the balance of Cu.
The invention also provides a preparation method of the copper wire with good conductivity, which comprises the following steps:
s1, preparing Ag-Cu alloy from Ag, Cu and La;
s2, coarsely crushing the Ag-Cu alloy and the Mg-Ca alloy into particles, uniformly mixing the Ag-Cu alloy particles, the raw material Le and the raw material Pb, putting the mixture into a smelting furnace, controlling the temperature rise when the temperature of the smelting furnace is raised to 1100-1200 ℃, putting the Mg-Ca alloy particles, and performing electromagnetic stirring for 2-6 min to prepare a liquid alloy;
s3, conveying the liquid alloy into casting equipment for casting to obtain a silver-copper alloy rod;
s4, mixing benzotriazole in an amount of 0.001-0.006: 1, adding the water-material ratio into ethanol, stirring and dissolving to obtain a passivation solution, soaking the silver-copper alloy rod into the passivation solution for 30-60 min, taking out and drying to obtain a silver-copper alloy rod subjected to surface treatment;
and S5, threading the silver-copper alloy rod obtained in the step S4 through a wire drawing machine for wire drawing, and annealing after wire drawing to obtain a finished product.
Preferably, the content of Ca in the Mg-Ca alloy is 1.5-2.2 wt%.
Preferably, the preparation of the Ag-Cu alloy comprises:
the method comprises the following steps of (1) granulating raw materials Ag and Cu coarse powder, carrying out high-energy ball milling on the Ag particles, the Cu particles and the La powder in a nitrogen atmosphere, wherein a ball milling medium is absolute ethyl alcohol, and carrying out ball milling to obtain a first processing material;
and (3) cold-pressing and molding the first processing material at the pressure of 200-490 MPa, carrying out heat preservation and sintering at the temperature of 635-800 ℃ in an argon atmosphere, and then, carrying out furnace cooling and taking out to obtain the La refined Ag-Cu alloy, wherein the heat preservation and sintering time is 2-4 h.
Preferably, in step S4, the passivation solution further includes urea and nitrite, and the ratio of benzotriazole to urea to nitrite is 1: 0.5-1: 0.2 to 1.
Compared with the prior art, the invention has the advantages that:
1. copper and silver are compounded to prepare a copper-based alloy, the conductivity of the material is increased, lanthanum is added in the compounding process, the lanthanum interacts with inevitable impurities in the copper and the silver to form an insoluble high-melting-point binary or multi-element compound, the distortion is weakened, crystals become more compact and regular to reduce the resistivity of the alloy, and the Mg-Ca alloy, the lead and the lithium act together to further increase the density and increase the mechanical property of the alloy, the thermal brittleness of the lead is eliminated by the action of the lanthanum and the lithium, so that the mechanical property of the lead is not weakened while the resistivity is reduced, and the corrosion resistance of the material is increased by the synergistic effect of benzotriazole and the lanthanum and the Mg-Ca alloy;
2. the material is more compact by firstly compounding copper and silver to prepare alloy and then crushing, the heat damage of the copper and the silver is reduced, and the mechanical property of the material is improved;
because magnesium and calcium are both active metals, the Mg-Ca alloy is put into the smelting furnace after Ag-Cu alloy particles, the raw material Le and the raw material Pb are smelted, so that the consumption of the Mg-Ca alloy in the smelting process is reduced;
and the Mg-Ca alloy is added and then is electromagnetically stirred, so that the turbulent motion is caused, the formation of fibrous and honeycomb structures is promoted, the compactness and the continuity of the material are not damaged, crystal grains are refined, the mechanical property of the material is improved, and the resistivity is reduced.
Detailed Description
The invention is further described below with reference to specific preferred embodiments, without thereby limiting the scope of protection of the invention.
Comparative example 1:
a copper wire with good conductivity comprises the basic components of 11 percent of Ag, 0.08 percent of Mg-Ca alloy, 0.03 percent of La, 1.5 percent of Le, 0.04 percent of Pb and the balance of Cu in percentage by weight; the copper wire comprises the following steps:
s1, preparing a raw material Ag and a raw material Cu into an Ag-Cu alloy;
s2, coarsely crushing the Ag-Cu alloy and the Mg-Ca alloy into particles, uniformly mixing the Ag-Cu alloy particles, the raw material Le and the raw material Pb, putting the mixture into a smelting furnace, controlling the temperature rise when the temperature of the smelting furnace is raised to 1100 ℃, putting the Mg-Ca alloy particles, and performing electromagnetic stirring for 6min to prepare liquid alloy;
s3, conveying the liquid alloy into casting equipment for casting to obtain a silver-copper alloy rod;
s4, placing the silver-copper alloy rod into ethanol, soaking for 50min, taking out, and airing to obtain the silver-copper alloy rod subjected to surface treatment;
and S5, threading the silver-copper alloy rod obtained in the step S4 through a wire drawing machine for wire drawing, and annealing after wire drawing to obtain a finished product.
Example 1:
the basic components comprise, by weight, 11% of Ag, 0.08% of Mg-Ca alloy, 0.03% of La, 1.5% of Le, 0.04% of Pb and the balance of Cu; the copper wire comprises the following steps:
s1, preparing a raw material Ag and a raw material Cu into an Ag-Cu alloy;
s2, coarsely crushing the Ag-Cu alloy and the Mg-Ca alloy into particles, uniformly mixing the Ag-Cu alloy particles, the raw material Le and the raw material Pb, putting the mixture into a smelting furnace, controlling the temperature rise when the temperature of the smelting furnace is raised to 1200 ℃, putting the Mg-Ca alloy particles, and performing electromagnetic stirring for 3min to prepare a liquid alloy;
s3, conveying the liquid alloy into casting equipment for casting to obtain a silver-copper alloy rod;
s4, adding benzotriazole into the mixture according to the weight ratio of 0.004: 1, adding the water-material ratio into ethanol, stirring and dissolving to obtain a passivation solution, soaking the silver-copper alloy rod into the passivation solution for 30min, taking out and drying to obtain a silver-copper alloy rod subjected to surface treatment;
and S5, threading the silver-copper alloy rod obtained in the step S4 through a wire drawing machine for wire drawing, and annealing after wire drawing to obtain a finished product.
Example 2:
the basic components comprise, by weight, 11% of Ag, 0.08% of Mg-Ca alloy, 0.03% of La, 1.5% of Le, 0.04% of Pb and the balance of Cu; the copper wire comprises the following steps:
s1, preparing a raw material Ag and a raw material Cu into an Ag-Cu alloy;
s2, coarsely crushing the Ag-Cu alloy and the Mg-Ca alloy into particles, uniformly mixing Ag-Cu alloy particles with the Ca content of 2.2 wt%, the raw material Le and the raw material Pb, putting the mixture into a smelting furnace, controlling the temperature rise when the temperature of the smelting furnace is raised to 1150 ℃, putting the Mg-Ca alloy particles, and performing electromagnetic stirring for 4min to prepare liquid alloy;
s3, conveying the liquid alloy into casting equipment for casting to obtain a silver-copper alloy rod;
s4, mixing benzotriazole in a proportion of 0.005: 1, adding the water-material ratio into ethanol, stirring and dissolving to obtain a passivation solution, soaking the silver-copper alloy rod into the passivation solution for 40min, taking out and drying to obtain a silver-copper alloy rod subjected to surface treatment;
and S5, threading the silver-copper alloy rod obtained in the step S4 through a wire drawing machine for wire drawing, and annealing after wire drawing to obtain a finished product.
Example 3:
the basic components comprise, by weight, 11% of Ag, 0.08% of Mg-Ca alloy, 0.03% of La, 1.5% of Le, 0.04% of Pb and the balance of Cu; the copper wire comprises the following steps:
s1, granulating a raw material Ag and a raw material Cu coarse powder, carrying out high-energy ball milling on the Ag particles, the Cu particles and the La powder in a nitrogen atmosphere, wherein a ball milling medium is absolute ethyl alcohol, and carrying out ball milling to obtain a first treatment material;
the first processing material is subjected to cold press molding under 390MPa pressure, is subjected to heat preservation sintering at 700 ℃ in argon atmosphere, is taken out in a furnace for cooling, and the La refined Ag-Cu alloy is obtained, wherein the heat preservation sintering time is 3 hours;
s2, roughly crushing the La refined Ag-Cu and Mg-Ca alloy into particles, uniformly mixing Ag-Cu alloy particles with the Ca content of 2.1 wt%, the raw material Le and the raw material Pb, putting the mixture into a smelting furnace, controlling the temperature rise when the temperature of the smelting furnace is raised to 1150 ℃, putting the Mg-Ca alloy particles into the smelting furnace, and performing electromagnetic stirring for 4min to obtain liquid alloy;
s3, conveying the liquid alloy into casting equipment for casting to obtain a silver-copper alloy rod;
s4, mixing benzotriazole in a proportion of 0.005: 1, adding the water-material ratio into ethanol, stirring and dissolving to obtain a passivation solution, soaking the silver-copper alloy rod into the passivation solution for 40min, taking out and drying to obtain a silver-copper alloy rod subjected to surface treatment;
and S5, threading the silver-copper alloy rod obtained in the step S4 through a wire drawing machine for wire drawing, and annealing after wire drawing to obtain a finished product.
Example 4
The basic components comprise, by weight, 11% of Ag, 0.08% of Mg-Ca alloy, 0.03% of La, 1.5% of Le, 0.04% of Pb and the balance of Cu; the copper wire comprises the following steps:
s1, granulating a raw material Ag and a raw material Cu coarse powder, carrying out high-energy ball milling on the Ag particles, the Cu particles and the La powder in a nitrogen atmosphere, wherein a ball milling medium is absolute ethyl alcohol, and carrying out ball milling to obtain a first treatment material;
the first processing material is subjected to cold press molding under 390MPa pressure, is subjected to heat preservation sintering at 700 ℃ in argon atmosphere, is taken out in a furnace for cooling, and the La refined Ag-Cu alloy is obtained, wherein the heat preservation sintering time is 3 hours;
s2, roughly crushing the La refined Ag-Cu and Mg-Ca alloy into particles, uniformly mixing Ag-Cu alloy particles with the Ca content of 2.1 wt%, the raw material Le and the raw material Pb, putting the mixture into a smelting furnace, controlling the temperature rise when the temperature of the smelting furnace is raised to 1150 ℃, putting the Mg-Ca alloy particles into the smelting furnace, and performing electromagnetic stirring for 4min to obtain liquid alloy;
s3, conveying the liquid alloy into casting equipment for casting to obtain a silver-copper alloy rod;
s4, mixing benzotriazole, urea and nitrite according to the proportion of 1: 0.8: 0.5 is added into ethanol, and the water-material ratio of the benzotriazole to the ethanol is 0.006: 1, stirring and dissolving to obtain a passivation solution, putting the silver-copper alloy rod into the passivation solution, soaking for 40min, taking out and drying to obtain a silver-copper alloy rod subjected to surface treatment;
and S5, threading the silver-copper alloy rod obtained in the step S4 through a wire drawing machine for wire drawing, and annealing after wire drawing to obtain a finished product.
The properties of the copper wire produced in comparative example 1 and examples 1 to 3 are shown in Table 1:
TABLE 1
The copper wires prepared in comparative example 1, example 1 and example 4 are respectively soaked in simulated seawater (3% NaCl aqueous solution) for 24 hours, the corrosion inhibition rate is analyzed, and the analysis results are shown in Table 2:
TABLE 2
| Comparative example 1 | Example 1 | Example 4 | |
| Sustained release rate (%) | 68.35 | 89.46 | 95.37 |
Please refer to tables 1 and 3, and the contents of the above comparative examples and examples, comparing comparative example 1 with example 1, it can be seen that comparative example 1 is prepared by first compounding Ag and Cu, and then melting them together with other materials, so that the material grains are finer and regular, and the resistivity of the material is reduced, but the resistivity of the common silver-copper material 1.78 × 10-8 Ω · m is not obviously different, and the hardness, the tensile strength and the corrosion resistance are not obviously improved, in example 1, on the basis of comparative example 1, lanthanum is added in the silver-copper compounding process, lanthanum, copper and unavoidable impurities in silver interact to form an insoluble high melting point binary or multi-element compound, distortion is reduced, the crystal becomes denser and regular, so as to reduce the resistivity of the alloy, and the Mg-Ca alloy, lead and lithium act together to further increase the compactness and increase the mechanical properties of the alloy, the lanthanum and the lithium act to eliminate the thermal brittleness of the lead, so that the mechanical property of the lead is not weakened while the resistivity of the lead is reduced, and the corrosion resistance of the material is improved due to the synergistic effect of the benzotriazole and the lanthanum and Mg-Ca alloy;
comparing example 1 with example 2, it can be seen that in example 2, the content of Ca in the Mg-Ca alloy is further limited based on example 1, when Ca is greater than 2.2 wt%, the average secondary dendrite of the alloy is significantly increased to form a continuous network structure, and the surrounding stress is increased during the deformation of the alloy, so that the mechanical property of the alloy is reduced, therefore, the content of Ca in the Mg-Ca alloy is limited in example 2, and the mechanical property and compactness of Mg are not affected while the activity of Mg is reduced;
comparing the embodiment 2 with the embodiment 3, it can be seen that the embodiment 3 further limits the preparation method of the Ag-Cu alloy on the basis of the embodiment 2, adopts a method of adding ethanol into a high-energy ball mill and introducing nitrogen, reduces the oxidation of the raw material Cu, and uses a cold pressing-sintering mode to prepare the Ag-Cu alloy at a low temperature, so that the mechanical property of the Ag-Cu alloy is increased, the oxidation consumption of the raw material Cu and the high-temperature smelting consumption of the raw materials Cu, Ag and La are reduced, the compactness of the material is further improved, and the mechanical property and the resistivity are relatively improved;
comparing example 3 with example 4, it is known that in example 3, on the basis of example 4, urea and nitrite are further added during the immersion of the passivation solution in step S4, so that the film forming property of the benzotriazole/ethanol solution is improved, and the corrosion resistance of the material is significantly increased.
As can be seen from the above, the copper wire obtained in example 4 has the best mechanical properties, resistivity and slow release rate compared with those of the copper wires obtained in examples 1 to 3, and therefore, example 4 is considered to be the most preferable example of the present invention.
The above description is only a preferred embodiment of the present invention, and the protection scope of the present invention is not limited to the above-described embodiments. All technical schemes belonging to the idea of the invention belong to the protection scope of the invention. It should be noted that modifications and embellishments within the scope of the invention may be made by those skilled in the art without departing from the principle of the invention, and such modifications and embellishments should also be considered as within the scope of the invention.
Claims (5)
1. A copper wire with good conductivity is characterized by comprising the following basic components in percentage by weight: 6 to 15 percent of Ag, 0.02 to 1 percent of Mg-Ca alloy, 0.02 to 0.045 percent of La, 1 to 3.3 percent of Le, 0.005 to 0.045 percent of Pb and the balance of Cu.
2. The method for preparing the copper wire with good conductivity according to claim 1, wherein the method comprises the following steps:
s1, preparing Ag-Cu alloy from Ag, Cu and La;
s2, coarsely crushing the Ag-Cu alloy and the Mg-Ca alloy into particles, uniformly mixing the Ag-Cu alloy particles, the raw material Le and the raw material Pb, putting the mixture into a smelting furnace, controlling the temperature rise when the temperature of the smelting furnace is raised to 1100-1200 ℃, putting the Mg-Ca alloy particles, and performing electromagnetic stirring for 2-6 min to prepare a liquid alloy;
s3, conveying the liquid alloy into casting equipment for casting to obtain an alloy rod with silver and copper;
s4, mixing benzotriazole in an amount of 0.001-0.006: 1, adding the water-material ratio into ethanol, stirring and dissolving to obtain a passivation solution, soaking the silver-copper alloy rod into the passivation solution for 30-60 min, taking out and drying to obtain a silver-copper alloy rod subjected to surface treatment;
and S5, threading the silver-copper alloy rod obtained in the step S4 through a wire drawing machine for wire drawing, and annealing after wire drawing to obtain a finished product.
3. The method for preparing the copper wire with good conductivity according to claim 2, wherein the content of Ca in the Mg-Ca alloy is 1.5-2.2 wt%.
4. The method for preparing the copper wire with good conductivity according to claim 2, wherein the preparation of the Ag-Cu alloy comprises the following steps:
the method comprises the following steps of (1) granulating raw materials Ag and Cu coarse powder, carrying out high-energy ball milling on the Ag particles, the Cu particles and the La powder in a nitrogen atmosphere, wherein a ball milling medium is absolute ethyl alcohol, and carrying out ball milling to obtain a first processing material;
and (3) cold-pressing and molding the first processing material at the pressure of 200-490 MPa, carrying out heat preservation and sintering at the temperature of 635-800 ℃ in an argon atmosphere, and then, carrying out furnace cooling and taking out to obtain the La refined Ag-Cu alloy, wherein the heat preservation and sintering time is 2-4 h.
5. The method for preparing the copper wire with good conductivity according to claim 2, wherein in the step S4, the passivating solution further comprises urea and nitrite, and the proportion of benzotriazole, urea and nitrite is 1: 0.5-1: 0.2 to 1.
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Application publication date: 20210709 |