CN108588471B - One-step synthesis method of copper-based electrode material containing nano zirconium carbide ceramic particles - Google Patents
One-step synthesis method of copper-based electrode material containing nano zirconium carbide ceramic particles Download PDFInfo
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- CN108588471B CN108588471B CN201810435441.2A CN201810435441A CN108588471B CN 108588471 B CN108588471 B CN 108588471B CN 201810435441 A CN201810435441 A CN 201810435441A CN 108588471 B CN108588471 B CN 108588471B
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- 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
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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
- C22C1/10—Alloys containing non-metals
- C22C1/1036—Alloys containing non-metals starting from a melt
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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
- C22C1/10—Alloys containing non-metals
- C22C1/1036—Alloys containing non-metals starting from a melt
- C22C1/1047—Alloys containing non-metals starting from a melt by mixing and casting liquid metal matrix composites
- C22C1/1052—Alloys containing non-metals starting from a melt by mixing and casting liquid metal matrix composites by mixing and casting metal matrix composites with reaction
Abstract
The invention belongs to the field of preparation of copper-based composite materials for welding electrodes, and discloses a one-step synthesis method of a copper-based electrode material containing nano zirconium carbide ceramic particles, which comprises the following steps: cold pressing the evenly mixed Cu powder, Zr powder and C powder into a precast block, then putting the Cu-Zr-C powder pressed compact and oxygen-free copper into a vacuum induction smelting furnace, firstly heating at low temperature to promote the thermal explosion synthesis reaction of the pressed compact, then heating to melt the oxygen-free copper and wrap reaction products, and preparing the ceramic copper-based composite material containing nano zirconium carbide by heat preservation and magnetic stirring. The copper-based electrode material containing the nano zirconium carbide ceramic particles is prepared in one step, so that the production cost is reduced, the working procedures are simplified, the production efficiency is improved, and meanwhile, the ZrC particles are fine and are uniformly distributed in copper.
Description
Technical Field
The invention belongs to the field of preparation of copper-based composite materials for welding electrodes, is mainly used for electrode tips, electrode caps and the like of welding machines, and particularly relates to a one-step synthesis method of a copper-based electrode material containing nano zirconium carbide ceramic particles.
Background
Spot welding is widely used in automobile, instrument and aviation manufacturing industries, and because of the high temperature and high pressure effect often endured in service, the copper alloy electrode is easy to lose efficacy, thereby reducing the production efficiency and influencing the quality of welding spots. With the widespread use of automatic welding and welding robots in modern production, there is an urgent need to develop electrode materials having both excellent electrical conductivity and mechanical properties. One of the effective ways to solve the problem of insufficient performance of copper alloy is to prepare a nano ceramic particle reinforced Cu-based composite material. The existing research shows that the nano Al2O3The particle reinforced Cu-based composite material has good mechanical properties, but Al2O3The ceramic is almost insulating (resistivity: 1020X 10)-6Ω · m), its introduction into the copper base significantly reduces the conductivity of the electrode. In contrast, ZrC has the advantages of high hardness (2560HV), high melting point (3540 ℃), good chemical stability (antioxidant temperature: 1100-1400 ℃) and thermal conductivity, and especially has outstanding electrical conductivity (resistivity: 0.42 × 10 ℃)-6Ω · m). Therefore, the addition of the nano ZrC ceramic in the copper matrix is expected to improve the mechanical property of the copper while maintaining the excellent conductivity of the copper.
At present, the main preparation method of the ZrC ceramic reinforced copper-based composite material comprises the following steps: (1) hot pressing sintering, i.e. sintering a mixture of Cu powder and ZrC powder at high temperature and high pressure for a long time (M.L Lopez, J.A. Jimez, D.Corredox. precipitation string high string h-reduction polymerization catalysis contacting ZrC ceramics, composites Part A: Applied Science and manufacturing.2007,38: 272) to obtain a mixture of Cu powder and ZrC powder. (2) The atmosphere sintering method is to sinter the mixed powder compacts of ZrC, Cu and the like after cold press molding in a protective atmosphere, and then prepare the composite material through the working procedures of extrusion, rolling and the like (Chinese patent application 201610437097.1, zirconium carbide copper-based contact material for low-voltage electrical appliances and a processing method thereof). (3) Self-propagating high temperature synthesis, i.e. a method of synthesizing ZrC/Cu by self-heating and self-conduction of high chemical reaction heat by igniting the exothermic reaction at one end of a mixed powder compact by an external heat source (Zhang M.X, Huang B, Hu Q.D et al. study of formatting floor of ZrC in the Cu-Zr-C system dual ceramic synthetic. International Journal of Refractory Metals and Hard materials.2012,31: 230-. The method has the problems of high energy consumption, high production cost, low efficiency, poor material conductivity, high material porosity and the like. Therefore, a more suitable method for preparing the ZrC/Cu composite material is required.
The invention provides a one-step synthesis method of a copper-based electrode material containing nano zirconium carbide ceramic particles, which is simple to operate, convenient to control, good in product conductivity and low in porosity.
Disclosure of Invention
In view of the technical problems in the prior art, the invention provides a one-step synthesis method of a copper-based electrode material containing nano zirconium carbide ceramic particles, which can improve the mechanical property of copper on the premise of keeping the excellent conductivity of the copper, and can effectively solve the problem of high price of nano zirconium carbide powder.
The invention provides a one-step synthesis method of a copper-based electrode material containing nano zirconium carbide ceramic particles, which comprises the following steps:
the method comprises the following steps of firstly, raw materials of Cu powder, Zr powder and C powder, wherein the molar ratio of the Zr powder to the C powder is 1, and the addition amount of the Cu powder is 10-60 wt.%;
step two, mixing the weighed Cu powder, Zr powder and C powder for 10-14 hours in an inert gas environment by using a roller ball mill to obtain Cu-Zr-C mixed powder;
step three, cold-pressing the mixed Cu-Zr-C powder into a pressed blank with the relative density of 50-70% by using a hydraulic press;
putting the Cu-Zr-C powder pressing block and the oxygen-free copper block into a vacuum induction smelting furnace, and then arranging the vacuum induction smelting furnace into a vacuum environment;
step five, preheating to 950-1050 ℃ through an induction coil of a smelting furnace in a vacuum environment so as to promote the thermal explosion synthesis reaction of the powder pressing block and the generation of ZrC ceramics, and then preserving heat for about 1 min;
and sixthly, continuously heating to 1250-1300 ℃, then preserving heat for 20-30min and applying magnetic stirring to uniformly disperse ZrC particles in the thermal explosion synthetic product in the Cu liquid, and finally casting the liquid into a metal mold to obtain the copper-based composite material containing the nano zirconium carbide ceramic particles.
The purity of the Cu powder is more than 99%, and the particle size is 0.5-75 mu m.
The Zr powder has the purity of more than 98 percent and the grain diameter of 45 mu m.
The purity of the C powder is more than 99%, and the particle size is 100 nm-1.3 mu m.
The oxygen-free copper block has a purity of 99.97%, an oxygen content of less than 0.003% and a total impurity content of no more than 0.03%.
The grinding balls of the ball mill are ZrO2Grinding balls, ZrO2The diameter of the grinding ball is 8mm, the weight ratio of the grinding ball to the powder is 10:1, and the rotating speed of the ball mill is 50-70 r/min.
The purity of the Ar gas is 99.999%.
The metal mold is an alloy steel mold.
The current of the magnetic stirring is 40-60A.
In the prepared copper-based electrode material containing the zirconium carbide ceramic particles, the size of ZrC particles is less than 100nm, the content is 0.1-1.0 wt%, and the balance is Cu.
In the first step, the molar ratio of Zr powder to C powder in the Cu-Zr-C mixed powder is 1, otherwise, the reaction is incomplete, and unreacted C or a byproduct Cu-Zr compound can be remained in the thermal explosion synthetic product.
And in the second step, the powder and the grinding balls are filled into a ball milling tank in an inert gas environment to prevent the powder such as Zr and the like from being oxidized in the mechanical ball milling process.
In the fourth step, the arrangement process of the vacuum environment is as follows: vacuumizing a smelting furnace to 5-10 Pa; and then injecting Ar gas to 0.06-0.08 MPa, repeatedly exhausting and inflating for three times, thereby removing air in the smelting furnace and preventing the Zr powder and the Cu powder from being oxidized in the heating process.
And fifthly, preheating to 950-1050 ℃ through an induction coil of a smelting furnace in a vacuum environment, and preserving heat for about 1min after the Cu-Zr-C powder pressed compact is subjected to thermal explosion reaction to generate ZrC ceramic, so that impurity gas is fully volatilized.
In the sixth step, the smelting temperature is 1250-1300 ℃, the heat preservation time and the magnetic stirring time are 20-30min, the applied magnetic stirring current is 40-60A, and ZrC in the thermal explosion synthetic product can be uniformly dispersed in the copper liquid under the action of high-temperature strong stirring for a long time.
In the invention, Cu powder is very important for the thermal explosion synthesis of the nano ZrC. Firstly, in the heating process, Cu and Zr can form Cu through solid-state diffusion reaction at 600-660 DEG C10Zr7Compounds of the same kind, with increasing temperature, Cu10Zr7The Zr powder and the C powder are dissolved into the Cu-Zr liquid phase, Zr and C atoms are combined into stable ZrC ceramic particles through rapid movement when the Zr powder and the C powder are dissolved into the Cu-Zr liquid phase, and therefore the ZrC thermal explosion synthesis reaction of the powder compact at 950-1050 ℃ is promoted. Second, after ZrC is formed from the liquid, the Cu liquid increases the distance between ZrC particles, thereby inhibiting contact and growth of the ZrC particles. Thirdly, Cu plays a role of a diluent, and the addition of Cu powder in the Zr-C mixed powder inevitably reduces the amount of Zr and C in unit volume, reduces the heat released by the formation of ZrC, further reduces the reaction temperature and inhibits the growth of ZrC.
In the invention, the smelting temperature (1250-1300 ℃) and the strong magnetic stirring (time 20-30min, current 40-60A) at the temperature are important for maintaining the nanometer state and the uniform distribution of ZrC in the composite material. If the smelting temperature is too low, the magnetic stirring time is too short and the current is too small, the magnetic stirring effect is reduced, so that the agglomeration of ZrC particles in the composite material is caused; when the temperature is too high and the magnetic stirring time is too long, ZrC particles in the composite material grow up and the segregation phenomenon occurs in the subsequent casting and cooling process.
The smelting process is adopted to prepare the copper-based electrode material containing the nano zirconium carbide ceramic particles, and compared with the sintering process, the copper-based electrode material has the following advantages that: (1) the cost is low; the sintering process can only be prepared by adopting a large amount of Cu powder and ZrC powder (or Zr powder and C powder), but the invention only needs a small amount of Cu powder, Zr powder, C powder and a large amount of Cu blocks, wherein the Cu blocks are cheap and much easier to obtain compared with Cu; (2) the product has low porosity and good conductivity; the sintering process is usually heated to a semi-molten state, namely the temperature cannot be higher than the melting point of Cu, pores of the powdery material are not completely removed, but if the temperature is higher than the melting point of Cu, the phenomenon of uneven distribution caused by different gravity is easy to occur, and the product has poor conductivity; the smelting temperature of the invention is higher than the melting point of Cu, and the magnetic stirring technology is adopted, thus not only removing pores, but also promoting the material to be uniformly distributed; (3) is suitable for large-scale production; the sintering process usually needs heat preservation and pressure of dozens of MPa is applied for sintering, and is suitable for preparing small products; the invention adopts the copper block as the raw material and can be used for large-scale production. The invention opens up a new idea for preparing the copper-based electrode material containing the nano zirconium carbide ceramic particles, and compared with the prior art, the invention has the following beneficial effects: (1) the Cu-Zr-C mixed powder is utilized to be thermally exploded to synthesize Cu-containing superfine ZrC powder, the price of the Cu-Zr-C mixed powder is lower than that of commercial superfine ZrC powder, and the preparation cost of the ZrC/Cu composite material can be reduced; (2) the preparation of ZrC particles and ZrC/Cu composite materials is realized in sequence in the heating process, and the additional preparation process of ZrC ceramic is simplified by a one-step method; (3) besides the dispersion strengthening effect, the nanometer ZrC ceramic particles can promote the refinement of a copper matrix through heterogeneous nucleation, realize fine-grain strengthening and improve the mechanical property of copper.
Drawings
Fig. 1 shows the microstructure of 0.2 wt.% of the nano copper zirconium carbide-based electrode material after corrosion in example 2 of the present invention.
Detailed Description
In order to make the technical means, the working procedures and the functions of the present invention easier to understand, the following embodiments are further described.
Example 1
The one-step synthesis method of the copper-based electrode material containing the nano zirconium carbide ceramic particles comprises the following steps:
1. weighing: cu powder with the grain diameter of 0.5 mu m, Zr powder with the grain diameter of 45 mu m and C powder with the grain diameter of 100nm are mixed according to the mol ratio of 0.4: 1: 1 weighing raw materials, wherein the raw materials are all commercial powder.
2. Mixing materials: putting the weighed Cu powder, Zr powder and C powder, grinding balls and a ball milling tank into a vacuum glove box, filling argon to normal pressure after vacuumizing to 5-10 Pa, putting the grinding balls and the powder into the ball milling tank in an inert gas environment, and then putting the sealed ball milling tank into a roller ball mill for mixing for 10 hours to obtain Cu-Zr-C mixed powder, wherein the grinding balls are ZrO2The weight ratio of the grinding balls to the powder is 10:1, and the rotating speed of the ball mill is 60 r/min.
3. Molding: the Cu-Zr-C mixed powder was put into a steel mold and then cold-pressed into a green compact having a relative density of about 65% by a hydraulic press.
4. Charging: mixing a Cu-Zr-C powder compact and an oxygen-free copper block according to the weight ratio of 1: 799 and then vacuum-pumping to about 5Pa, then charging Ar gas to 0.06-0.08 MPa, and repeatedly pumping and charging gas for three times.
5. Synthesizing: in a vacuum environment, the temperature is raised to about 980 ℃ through an induction coil of a smelting furnace, the thermal explosion synthesis reaction of the Cu-Zr-C powder compact is promoted, and then the temperature is kept for about 1 min.
6. And smelting: and continuously heating to 1250 ℃, then preserving heat for 30min, starting magnetic stirring, applying 40A stirring current, finally closing a heating power supply and a magnetic stirring power supply, and casting the liquid into a metal mold to obtain the 0.1 wt.% copper-based electrode material of the nano zirconium carbide ceramic particles. The tensile strength of the composite material was 308MPa, and the electrical conductivity was 97% IACS.
Example 2
The one-step synthesis method of the copper-based electrode material containing the nano zirconium carbide ceramic particles was the same as in example 1 except for the following.
In this embodiment:
(1) in the Cu-Zr-C mixed powder, Cu powder, Zr powder and C powder are mixed according to a molar ratio of 0.69: 1: 1, weighing;
(2) the weight ratio of the oxygen-free copper block to the Cu-containing nano ZrC powder is 349: 1, putting the mixture into a vacuum smelting furnace;
(3) 0.2 wt.% of the copper-based electrode material of the nano zirconium carbide ceramic particles is obtained. The tensile strength of the composite material is 356MPa, and the electric conductivity is 95% IACS.
Fig. 1 is a microstructure of 0.2 wt.% of a nano copper zirconium carbide based electrode material after corrosion. As can be seen from FIG. 1.a, ceramic particles having a size of less than 100nm are uniformly distributed in a Cu matrix. FIG. 1.b is the energy spectrum of the selected region (within the box). It can be seen that this region is composed of three elements, Cu, Zr, and C, indicating that the ceramic particle is ZrC.
Example 3
The one-step synthesis method of the copper-based electrode material containing the nano zirconium carbide ceramic particles was the same as in example 1 except for the following.
In this embodiment:
(1) the grain size of Cu powder in the Cu-Zr-C mixed powder is 75 mu m;
(2) the weight ratio of the oxygen-free copper block to the Cu-Zr-C powder compact is 79: 1, putting the mixture into a vacuum smelting furnace;
(3) keeping the temperature and magnetically stirring for 20min, and controlling the magnetic stirring current to be 60A;
(4) obtaining 1.0 wt.% of the copper-based electrode material of the nano zirconium carbide ceramic particles. The tensile strength of the composite material was 483MPa, and the electrical conductivity was 85% IACS.
Example 4
The one-step synthesis method of the copper-based electrode material containing the nano zirconium carbide ceramic particles was the same as in example 1 except for the following.
In this embodiment:
(1) the particle size of C powder in the Cu-Zr-C mixed powder is 1.3 mu m, and the molar ratio of Cu powder, Zr powder and C powder is 0.18: 1: 1, weighing Cu-Zr-C powder, mixing for 14 hours by using a ball mill, wherein the rotating speed of the ball mill is 50 revolutions per minute, and cold-pressing into a pressed blank with the relative density of 50%;
(2) the synthesis temperature of the Cu-Zr-C powder compact is 950 ℃;
(3) the melting temperature was 1300 ℃.
Example 4
The one-step synthesis method of the copper-based electrode material containing the nano zirconium carbide ceramic particles was the same as in example 1 except for the following.
In this embodiment:
(1) in the Cu-Zr-C mixed powder, Cu powder, Zr powder and C powder are mixed according to a molar ratio of 2.4: 1: 1, weighing; the rotating speed of the ball mill is 70 r/min;
(2) cold-pressing the Cu-Zr-C mixed powder into a pressed compact with the relative density of 70%;
(3) the synthesis temperature of the Cu-Zr-C powder compact was 1050 ℃.
Claims (6)
1. The one-step synthesis process of copper-base electrode material containing nanometer zirconium carbide ceramic particle includes the following steps:
the method comprises the following steps of firstly, raw materials of Cu powder, Zr powder and C powder, wherein the molar ratio of the Zr powder to the C powder is 1, and the addition amount of the Cu powder is 10-60 wt.%;
step two, mixing the weighed Cu powder, Zr powder and C powder for 10-14 hours in an inert gas environment by using a roller ball mill to obtain Cu-Zr-C mixed powder;
step three, cold-pressing the mixed Cu-Zr-C powder into a pressed blank with the relative density of 50-70% by using a hydraulic press;
putting the Cu-Zr-C powder pressing block and the oxygen-free copper block into a vacuum induction smelting furnace, and then arranging the vacuum induction smelting furnace in a vacuum environment;
step five, preheating to 950-1050 ℃ through an induction coil of a smelting furnace in a vacuum environment, so as to promote the thermal explosion synthesis reaction of the powder precast block and the synthesis of ZrC ceramic, and then preserving heat for about 1 min;
step six, continuously heating to 1250-1300 ℃ to melt the oxygen-free copper, then preserving heat for 20-30min and applying magnetic stirring to uniformly disperse the ZrC particles synthesized by thermal explosion in oxygen-free copper liquid, and finally casting the liquid into a metal mold to obtain the copper-based electrode material containing the nano zirconium carbide ceramic particles;
in the copper-based electrode material containing the zirconium carbide ceramic particles, the content of ZrC particles is 0.1-1.0 wt%, and the balance is Cu.
2. The one-step synthesis method of copper-based electrode material containing nano zirconium carbide ceramic particles according to claim 1, wherein in the second step, the grinding balls of the ball mill are ZrO2Grinding balls, ZrO2Diameter of grinding ballThe grinding ball mill is 8mm, the weight ratio of the grinding balls to the powder is 10:1, and the rotating speed of the ball mill is 50-70 r/min.
3. The one-step synthesis method of the copper-based electrode material containing the nano zirconium carbide ceramic particles according to claim 1, wherein in the fourth step, the arrangement process of the vacuum environment comprises the following steps: vacuumizing a smelting furnace to 5-10 Pa; then, Ar gas is injected to 0.06-0.08 MPa, and the air is repeatedly pumped and inflated for three times.
4. The one-step synthesis method of the copper-based electrode material containing the nano zirconium carbide ceramic particles according to claim 1, wherein the Cu powder has a purity of more than 99% and a particle size of 0.5-75 μm, the Zr powder has a purity of more than 98% and a particle size of 45 μm, and the C powder has a purity of more than 99% and a particle size of 100 nm-1.3 μm.
5. The one-step synthesis method of the copper-based electrode material containing the nano zirconium carbide ceramic particles according to claim 1, wherein in the sixth step, the applied magnetic stirring current is 40-60A.
6. The one-step synthesis method of the copper-based electrode material containing the nano zirconium carbide ceramic particles as claimed in claim 1, wherein the size of ZrC particles in the copper-based electrode material containing the nano zirconium carbide ceramic particles is less than 100 nm.
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| CN109722560B (en) * | 2018-12-03 | 2020-09-08 | 江西理工大学 | ZrC reinforced Cu-Fe-based composite material and preparation method thereof |
| CN110504113A (en) * | 2019-08-21 | 2019-11-26 | 哈尔滨东大高新材料股份有限公司 | A kind of addition zircon powder ZrSiO4Strengthen copper-based electrical contact material |
| CN111468801B (en) * | 2020-04-21 | 2022-02-01 | 南昌航空大学 | Method for planting precise pulse arc spot welding ceramic particles |
| CN112375926A (en) * | 2020-11-10 | 2021-02-19 | 将乐三晶新材料有限公司 | Process equipment system for producing silicon-zirconium-aluminum alloy |
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