CN108531767B - Preparation method of superfine zirconium carbide particle dispersion-strengthened copper-based composite material for spot welding electrode - Google Patents
Preparation method of superfine zirconium carbide particle dispersion-strengthened copper-based composite material for spot welding electrode Download PDFInfo
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Abstract
The invention belongs to the field of preparation of copper-based composite materials for welding electrodes, and discloses a preparation method of a superfine zirconium carbide particle dispersion-strengthened copper-based composite material for spot welding electrodes, which comprises the following steps: and (2) cold-pressing and molding the uniformly mixed Cu-Zr-C powder, putting the powder pressed compact into self-propagating high-temperature synthesis equipment for ignition to obtain Cu-containing superfine ZrC powder, smelting a mixture of oxygen-free copper and the Cu-containing superfine ZrC powder in a vacuum smelting furnace, and magnetically stirring to prepare the superfine ZrC particle dispersion-strengthened copper-based composite material. The method has the characteristics of low cost, simple process, high production efficiency, small ZrC size, uniform distribution and the like.
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 preparation method of a superfine zirconium carbide particle dispersion-strengthened copper-based composite material for spot welding electrodes.
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. Solve the problem of insufficient performance of copper alloyOne effective way is to prepare the superfine 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 superfine ZrC 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 preparation method of a superfine zirconium carbide particle dispersion strengthening copper-based composite material for a spot welding electrode, which is simple to operate, convenient to control, high in product hardness and low in porosity.
Disclosure of Invention
In view of the technical problems in the prior art, the invention provides a preparation method of a superfine zirconium carbide particle dispersion-strengthened copper-based composite material for a spot welding electrode, which can improve the mechanical property of copper on the premise of keeping the excellent conductivity of the copper, and effectively solves the problem of high price of superfine zirconium carbide powder.
The invention provides a preparation method of a superfine zirconium carbide particle dispersion strengthening copper-based composite material for a spot welding electrode, which comprises the following steps:
taking Cu powder, Zr powder and graphite powder as raw materials to prepare a Cu-containing superfine ZrC product;
grinding the expanded and loose Cu-containing superfine ZrC product into powder;
putting the Cu-containing superfine ZrC powder and the copper foil into a glove box, and then sealing the Cu-containing ZrC powder by using the copper foil in an inert gas environment;
putting the Cu-containing superfine ZrC powder sealed by the oxygen-free copper block and the copper foil into a vacuum smelting furnace, wherein the Cu-containing superfine ZrC powder sealed by the copper foil is placed below the oxygen-free copper block; and after vacuum pumping, heating a smelting furnace to 1200-1250 ℃ to melt the oxygen-free copper blocks and cover the surfaces of the Cu-containing superfine ZrC powder, then preserving the heat for 5-10min, applying magnetic stirring to uniformly distribute ZrC particles in Cu liquid, and finally casting the Cu-based composite material into a metal mold to obtain the superfine ZrC particle dispersion strengthened Cu-based composite material.
The specific preparation process of the step one comprises the following steps:
step (1), taking Cu powder, Zr powder and graphite powder as raw materials, wherein the addition amount of the Cu powder is 40 wt.%, and the molar ratio of the Zr powder to the C powder is 1;
step (2), 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 (3), filling the Cu-Zr-C mixed powder into an alloy steel die, and pressing into a powder compact with relative density of 65 +/-5% by using a hydraulic press;
step (4), putting the Cu-Zr-C powder compact into self-propagating high-temperature synthesis equipment (glove box), and arranging the compact into an inert gas environment;
and (5) rapidly igniting a self-propagating high-temperature synthesis reaction at one end of the pressed compact through electric arc generated by a tungsten electrode, then immediately extinguishing the electric arc, and obtaining the expanded and loose Cu-containing superfine ZrC product after the combustion wave spontaneously propagates to the whole pressed compact.
The Cu powder has a purity of 99% and an average particle diameter of 0.5 μm.
The Zr powder has the purity of more than 98 percent and the grain diameter of 45 mu m.
The purity of the graphite powder is more than 99%, and the particle size is 100 nm.
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 not 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 20-30A.
In the prepared superfine ZrC particle dispersion strengthened Cu-based composite material, the size of ZrC particles is 100 nm-0.5 μm, the content is 0.1 wt.% to 1.0 wt.%, and the balance is Cu.
In the step (1), the Cu content in the Cu-Zr-C mixed powder is about 40 wt.%, and the molar ratio of Zr powder to C powder is 1; when the Cu content is too low, ZrC particles having a large size (several μm) are formed, and when the Cu content is too high or the molar ratio of Zr to C is not 1, the reaction is incomplete, and unreacted C and a by-product Cu-Zr compound remain in the product.
In the step (2), the powder and the grinding balls are filled into a ball milling tank in an inert gas environment to prevent the oxidation of the powder such as Zr in the mechanical ball milling process.
In the step (3), the relative density of the cold-pressed Cu-Zr-C mixed powder compact is about 65%, if the relative density is too low, the combustion wave is difficult to spread spontaneously to cause no reaction or incomplete reaction, and if the relative density is too high, micron-sized ZrC particles can be synthesized due to high combustion temperature.
In the step (4), the inert gas environment is arranged as follows: firstly, vacuumizing self-propagating high-temperature synthesis equipment to 5-10 Pa; then filling Ar gas to 0.06-0.08 MPa, and repeatedly pumping and filling air for three times; and finally, filling Ar gas into the self-propagating high-temperature synthesis equipment to normal pressure, thereby removing air in the equipment and preventing the oxidation of Zr in the self-propagating high-temperature synthesis process.
In the step (5), the graphite flake is rapidly heated by electric arc generated by the tungsten electrode, and is placed on the graphite and the lower surface of the powder pressed compact by utilizing high-temperature heating of the graphite flake, so that the self-propagating high-temperature synthesis reaction at one end of the pressed compact is ignited.
In the second step, the fluffy Cu-containing ZrC particles need to be ground into powder, so that the ZrC particles can be stirred and dispersed in the copper liquid in the subsequent smelting process.
And in the third step, placing the Cu-containing superfine ZrC powder and the copper foil into a glove box, vacuumizing to 5-10 Pa, filling argon to normal pressure, and sealing the Cu-containing ZrC powder by using the copper foil, so that the phenomenon that oxygen, water and the like in the air are adsorbed on the surface of the superfine ZrC powder is avoided. On the other hand, the powder is prevented from being sucked away in the subsequent smelting process and the vacuumizing stage.
In the fourth step, the Cu-containing superfine ZrC powder sealed by the copper foil is placed under an oxygen-free copper block to prevent ZrC particles from floating on the surface of copper liquid and aggregating after the copper is melted and before stirring; the smelting temperature is 1200-1250 ℃, the fluidity of the copper liquid is poor when the temperature is too low, the stirring effect is limited, and the ZrC particles are subjected to segregation phenomenon due to small specific gravity in the long-time cooling process after the copper liquid is cast into a mold when the temperature is too high; the applied magnetic stirring current is 20-30A, and the time is 5-10min, so as to ensure the dispersion distribution of the superfine ZrC in the copper.
In the invention, the Cu powder additive is used for preparing Cu-containing superfine ZrC powderIt is of great importance. 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 graphite powder are dissolved into the Cu-Zr liquid phase, Zr and C atoms are combined into stable ZrC ceramic particles through rapid movement, and thus the complete synthesis of ZrC 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 has good heat conductivity coefficient, so that the cooling rate of the reaction product in the cooling process can be increased, the retention time of the product at high temperature is reduced, and the growth of ZrC is prevented. Fourthly, 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 (1200-1250 ℃) and the magnetic stirring (5-10 min) at the temperature are important for maintaining the ZrC in the composite material in an ultrafine state and uniform distribution. If the smelting temperature is too low and the magnetic stirring time is too short, the magnetic stirring effect is reduced, so that the ZrC particles in the composite material are agglomerated; when the temperature is too high and the magnetic stirring time is too long, ZrC particles in the composite material grow up, and the phenomenon of segregation occurs in the subsequent standing and cooling process.
The invention opens up a new idea for preparing the superfine zirconium carbide particle dispersion strengthening copper-based composite material for the spot welding electrode, and compared with the prior art, the invention has the following beneficial effects: (1) the Cu-Zr-C mixed powder is used for self-propagating high-temperature synthesis of 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 Cu-containing superfine ZrC powder can be directly used for preparing copper-based composite materials, and the ZrC extraction process is omitted; (3) the ZrC/Cu composite material has simple preparation process, small ZrC particle size and uniform distribution; (4) besides the dispersion strengthening effect, the superfine ZrC particles in the ZrC/Cu composite material 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 XRD detection result of Cu-containing superfine ZrC powder in example 3 of the present invention;
FIG. 2 shows the etched morphology of the ultra-fine ZrC particle dispersion strengthened copper-based composite material in example 3 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
A preparation method of the superfine zirconium carbide particle dispersion strengthening copper-based composite material for the spot welding electrode comprises the following steps:
1. weighing: cu powder with the grain diameter of 0.5 mu m, Zr with the grain diameter of 45 mu m and graphite powder with the grain diameter of 100nm are mixed according to the mol ratio of 1.1: 1: 1 weighing raw materials, wherein the raw materials are all commercial powder.
2. Mixing materials: putting the weighed Cu powder, Zr powder, C powder, grinding balls and a ball milling tank into a vacuum glove box, vacuumizing to 5-10 Pa, filling argon to normal pressure, putting the grinding balls and the powder into the ball milling tank in an inert gas environment, and putting the sealed ball milling tank into a roller ball mill for mixing for 10 hours, wherein the grinding balls are ZrO2Grinding balls, wherein the weight ratio of the grinding balls to the powder is 10:1, and the rotating speed of the ball mill is 70 r/min;
3. molding: the Cu-Zr-C mixed powder is put into a steel die and then is cold-pressed into a green compact with the relative density of 65 +/-5 percent by a hydraulic press.
4. Charging: putting the Cu-Zr-C powder compact into self-propagating high-temperature synthesis equipment, pumping vacuum to 5-10 Pa, then filling Ar gas to 0.06-0.08 MPa, and repeatedly pumping and inflating for three times.
5. Igniting: ar gas is filled into self-propagating high-temperature synthesis equipment to normal pressure, electric arc is generated through a tungsten electrode of an in-equipment sub-arc welding machine, the graphite flake is rapidly heated by the high-temperature electric arc, when heat is transmitted to a powder pressed compact on the graphite flake from the graphite flake, the temperature of the bottom of the powder pressed compact is rapidly raised, once the bottom is ignited, the electric arc is immediately extinguished, a combustion wave upwards spontaneously propagates until the whole pressed compact reaction is finished, and the temperature is cooled to room temperature, so that the expanded and loose Cu-containing superfine ZrC product can be obtained.
6. Grinding: grinding the Cu-containing superfine ZrC product which is loose in expansion into powder.
7. Sealing: placing the Cu-containing superfine ZrC powder and the copper foil into a glove box, vacuumizing to 5-10 Pa, filling argon to normal pressure, and sealing the Cu-containing ZrC powder by using the copper foil.
8. Smelting: sealing an oxygen-free copper block and a copper foil to obtain Cu-containing superfine ZrC powder in a weight ratio of 599: 1, placing the copper foil sealed superfine ZrC powder containing Cu in a vacuum smelting furnace, wherein the copper foil sealed superfine ZrC powder containing Cu is placed below an oxygen-free copper block; vacuumizing the smelting furnace to about 5Pa by using a mechanical pump, and then heating the smelting furnace to 1200-1250 ℃ to melt the oxygen-free copper block and cover the surface of the Cu-containing superfine ZrC powder; then preserving the heat for 5min, starting a magnetic stirrer, and applying a stirring current of 20A to enable the ZrC powder and the copper liquid to rotate together for 5 min; and (3) turning off the heating power supply and the magnetic stirring power supply, casting the liquid into a metal mold, and cooling to room temperature to obtain the superfine ZrC/Cu composite material with the ZrC content of 0.1 wt.%. The tensile strength of the composite material was 268MPa, and the electrical conductivity was 98% IACS.
Example 2
A method for producing a copper-based composite material dispersion-strengthened with ultrafine zirconium carbide particles for a spot welding electrode, which was the same as in example 1, except for the following points.
In this embodiment:
(1) the rotating speed of the ball mill is 50 revolutions per minute; applying a magnetic stirring current of 30A;
(2) the weight ratio of the oxygen-free copper block to the Cu-containing superfine ZrC powder is 299: 1, putting the mixture into a vacuum smelting furnace;
(3) obtaining the superfine ZrC/Cu composite material with the ZrC content of 0.2 wt.%. The tensile strength of the composite material is 302MPa, and the electric conductivity is 96% IACS.
Example 3
A method for producing a copper-based composite material dispersion-strengthened with ultrafine zirconium carbide particles for a spot welding electrode, which was the same as in example 1, except for the following points.
In this embodiment:
(1) the rotating speed of the ball mill is 60 revolutions per minute; the weight ratio of the oxygen-free copper block to the Cu-containing superfine ZrC powder is 59: 1, putting the mixture into a vacuum smelting furnace;
(2) the magnetic stirring time is 10min, and the magnetic stirring current is 30A;
(3) obtaining the superfine ZrC/Cu composite material with the ZrC content of 1.0 wt.%. The tensile strength of the composite material was 414MPa, and the electrical conductivity was 90% IACS.
FIG. 1 shows the XRD detection result of Cu-containing superfine ZrC powder. As can be seen from FIG. 1, the Cu-containing ultrafine ZrC powder consisted of only two phases of ZrC and Cu, and no zirconia, unreacted Zr or C were detected, indicating that Zr and C were converted to ZrC.
FIG. 2 is the shape of the ultra-fine ZrC particle dispersion strengthened copper-based composite material after corrosion. As can be seen from the figure, the superfine ZrC particles are uniformly distributed in the Cu matrix, and the size of the ZrC particles is 100 nm-0.5 μm.
Claims (5)
1. A preparation method of superfine zirconium carbide particle dispersion strengthening copper-based composite material for spot welding electrodes comprises the following steps:
step one, preparing a Cu-containing superfine ZrC product by taking Cu powder, Zr powder and graphite powder as raw materials;
grinding the expanded and loose Cu-containing superfine ZrC product into powder;
putting the Cu-containing superfine ZrC powder and the copper foil into a glove box, and then sealing the Cu-containing ZrC powder by using the copper foil in an inert gas environment;
putting the Cu-containing superfine ZrC powder sealed by the oxygen-free copper block and the copper foil into a vacuum smelting furnace, wherein the Cu-containing superfine ZrC powder sealed by the copper foil is placed below the oxygen-free copper block; after vacuum pumping, heating a smelting furnace to 1200-1250 ℃, melting an oxygen-free copper block and covering the oxygen-free copper block on the surface of the Cu-containing superfine ZrC powder, then preserving heat for 5-10min, applying magnetic stirring to uniformly distribute ZrC in Cu liquid, and finally casting the Cu-containing superfine ZrC powder into a metal mold to obtain the superfine ZrC particle dispersion strengthened Cu-based composite material, wherein the applied magnetic stirring current is 20-30A, and the time is 5-10 min;
the specific preparation process of the step one comprises the following steps:
taking Cu powder, Zr powder and graphite powder as raw materials, wherein the molar ratio of the Zr powder to the C powder is 1, and the addition amount of the Cu powder is 40 wt.%;
step (2), 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 (3), filling the Cu-Zr-C mixed powder into an alloy steel die, and then cold-pressing the Cu-Zr-C powder into a pressed blank with the relative density of 65 +/-5% by using a hydraulic press;
step (4), putting the Cu-Zr-C powder compact into self-propagating high-temperature synthesis equipment, and arranging the compact into an inert gas environment;
and (5) igniting a self-propagating high-temperature synthesis reaction at one end of the pressed compact by using electric arc generated by a tungsten electrode, immediately extinguishing the electric arc, and spontaneously propagating a combustion wave to the whole pressed compact to obtain the expanded and loose Cu-containing superfine ZrC product.
2. The method for preparing the ultrafine zirconium carbide particle dispersion-strengthened copper-based composite material for the spot welding electrode according to claim 1, wherein in the step (2), the grinding ball of the ball mill is 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.
3. The method for preparing the superfine zirconium carbide particle dispersion strengthened copper-based composite material for the spot welding electrode according to the claim 1, wherein in the step (4), the inert gas environment is arranged as follows: firstly, vacuumizing a high-temperature atmosphere furnace to 5-10 Pa; then filling Ar gas to 0.06-0.08 MPa, and repeatedly pumping and filling air for three times; and finally, filling Ar gas into the self-propagating high-temperature synthesis equipment to normal pressure.
4. The method for preparing the ultrafine zirconium carbide particle dispersion-strengthened copper-based composite material for the spot welding electrode according to claim 1, wherein the Cu powder has a purity of > 99% and an average particle size of 0.5 μm, the Zr powder has a purity of > 98% and a particle size of 45 μm, and the graphite powder has a purity of > 99% and a particle size of 100 nm.
5. The method for preparing the superfine zirconium carbide particle dispersion-strengthened copper-based composite material for the spot welding electrode according to claim 1, wherein the size of the ZrC particles in the superfine ZrC particle dispersion-strengthened Cu-based composite material is 100nm to 0.5 μm, the content of the ZrC particles is 0.1 wt.% to 1.0 wt.%, and the balance is Cu.
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