CN111872517B - Mg-Zr intermediate alloy pretreatment method for improving magnesium alloy refinement effect - Google Patents
Mg-Zr intermediate alloy pretreatment method for improving magnesium alloy refinement effect Download PDFInfo
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- B23K—SOLDERING OR UNSOLDERING; WELDING; CLADDING OR PLATING BY SOLDERING OR WELDING; CUTTING BY APPLYING HEAT LOCALLY, e.g. FLAME CUTTING; WORKING BY LASER BEAM
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Abstract
The invention discloses a Mg-Zr intermediate alloy pretreatment method for improving the magnesium alloy refining effect, which comprises the step of carrying out multi-pass wire filling processing on a Mg-Zr intermediate alloy plate by using high-frequency pulse alternating current TIG welding, so that Zr particles are dispersed under the disturbance of high-frequency pulse current and are simultaneously dispersed and dissolved to form Zr solute atoms under the high-temperature environment of electric arc. The molten pool solidified on a water-cooled copper base, so that a large amount of Zr solute atoms were dissolved into the magnesium matrix. The pretreatment method not only realizes the conversion from large-particle Zr to small-particle Zr in the Mg-Zr intermediate alloy, but also realizes the conversion from small-particle Zr to solute atom Zr. The Mg-Zr intermediate alloy pretreated by the method has better magnesium alloy refining effect, longer decay time, short process flow and flexible and convenient operation.
Description
Technical Field
The invention belongs to the technical field of magnesium alloy, relates to a refining process method of a magnesium alloy solidification structure, and particularly relates to a Mg-Zr intermediate alloy pretreatment method for improving the magnesium alloy refining effect.
Background
Magnesium and magnesium alloy are the lightest metal structure materials applicable at present, have a series of advantages of low density, high specific strength and specific rigidity, excellent damping and shock absorbing performance, strong electromagnetic shielding performance and the like, and are widely applied in the fields of aerospace, ground transportation, 3C products and the like. According to the Hall-Peltier equation sigmay＝σ0+kyD-1/2K of magnesium alloyyThe value is higher, so that the improvement of the strength of the magnesium alloy through fine grain strengthening has important significance. At present, Zr is the most effective refiner for cast magnesium alloy without Al, Mn, Si and Fe. The addition of Zr can also reduce the heat cracking tendency of the magnesium alloy and improve the strength, the plastic toughness and the corrosion resistance of the alloy. When the addition amount of Zr is between 0.5 and 1.0 percent, fine equiaxed crystals can be obtained in the magnesium alloy. Zr usually exists in two forms in magnesium alloy, namely undissolved particlesZr and solute atoms Zr dissolved in the magnesium matrix. As Zr and Mg are in a close-packed hexagonal structure and the lattice constants of the Zr and the Mg are close, the particle Zr with a proper size can be used as a heterogeneous nucleation core of the Mg, and the nucleation rate can be improved in the solidification process to achieve the purpose of refining grains. Meanwhile, compared with other common alloy elements in magnesium, solute atom Zr has the strongest effect of inhibiting the growth of Mg dendrites, and the growth inhibition factor of the solute atom Zr on alpha-Mg dendrites is as high as 38.29. In other words, solute Zr refines the texture by creating a strong compositional supercooling effect.
Although both the granular Zr and the solute Zr have a certain refining effect on the magnesium alloy, a great deal of research proves that the solute Zr contributes better to grain refining than the granular Zr. Meanwhile, compared with solute Zr, the grain Zr is easy to be settled in magnesium melt due to the larger density difference between the grain Zr and Mg, so that the refining recession effect of the grain Zr is obvious. However, in the traditional Mg-Zr intermediate alloy, the Zr particles are obviously agglomerated, and the Zr particle size is generally larger. The large-size Zr particles are not easy to disperse and dissolve in the actual smelting process, but are precipitated due to the high density. Therefore, the traditional Mg-Zr intermediate alloy has poor refining effect on the magnesium alloy. Meanwhile, the yield of Zr is low due to the sedimentation of Zr particles, and the preparation cost of the alloy is improved. In order to improve the refining effect, prolong the refining decay time and reduce the production cost, the size refinement of the particle Zr and the transformation of the particle Zr to the solute Zr in the modes of diffusion, dissolution and the like are promoted by generally increasing the Zr adding temperature, prolonging the heat preservation time, applying melt stirring and the like in the actual casting production process. However, the retention time of the melt at high temperature is prolonged, and even stirring at high temperature can cause strong oxidation of the magnesium melt, which undoubtedly increases the difficulty of the subsequent refining process and reduces the preparation quality of the melt.
Therefore, a great deal of theoretical research and technical development is carried out in both academic circles and industrial circles, and the improvement of the Zr existing state in the Mg-Zr intermediate alloy is expected to improve the refining effect. Found by the literature search, Improvement in the sensitivity of the crystal grain of Mg-Zr master alloy for magnesium alloy by friction stir processingThinning effect) ("Journal of Magnesium and Alloys" 2014; 2: pp 239-244) describes that the grain refining effect of the Mg-Zr intermediate alloy is improved by performing friction stir processing pretreatment on the Mg-30 wt% Zr intermediate alloy to break and disperse large-size Zr particles. However, as a solid forming process, the stirring friction processing can only change the size of Zr particles, the crushing effect on the Zr particles is very limited, and FSP equipment is large in size, complex to operate and long in process flow. CN101798635A discloses a Zr composite cake made by smelting magnesium alloy and a preparation method thereof, wherein a layer of Zr salt cake is firstly placed in a two-layer coating salt cake to be processed into a composite cake through extrusion, and then the composite cake is pressed into a magnesium melt to be melted to generate a large amount of Zr solute atoms so as to achieve the refining effect. As the Zr salt can provide a large amount of solute Zr for the melt, the refining effect is much better than that of the Mg-Zr intermediate alloy. However, conventional Zr salts have been found to be very hygroscopic and the Zr salts that thicken in high temperature melts are often associated with MgF2And the reaction products are symbiotic, so that the wetting and capturing capacity of the conventional refining agent to slag inclusion is reduced, the purity of the melt is reduced, and the mechanical property and the corrosion property of the alloy are obviously deteriorated.
In conclusion, the current Mg-Zr intermediate alloy has limited refining effect and obvious refining recession effect on the magnesium alloy, and the main reason is that a large amount of Zr particles with larger sizes in the Mg-Zr intermediate alloy are easy to settle in the smelting process. Therefore, it is important to develop a novel pretreatment process of the Mg-Zr intermediate alloy to improve the existence state of Zr in the intermediate alloy and improve the refining effect of the intermediate alloy.
Disclosure of Invention
Aiming at the defects in the prior art, the invention aims to solve the problems of reduced refining effect and rapid refining decline caused by the sedimentation of Zr particles in the conventional Mg-Zr intermediate alloy due to the difficulty in dissolving the Zr particles in the smelting process, and provides a Mg-Zr intermediate alloy pretreatment method for improving the magnesium alloy refining effect. The Mg-Zr intermediate alloy pretreated by the method has better magnesium alloy refining effect, longer decay time, short process flow and flexible and convenient operation.
The purpose of the invention is realized by the following technical scheme:
the invention provides a Mg-Zr intermediate alloy pretreatment method for improving the magnesium alloy refining effect, which is characterized by comprising the step of carrying out multi-pass wire filling processing on a Mg-Zr intermediate alloy plate by using high-frequency pulse alternating current Tungsten Inert Gas (TIG) welding; the Zr particles can be dispersed under the disturbance of high-frequency pulse current, and can be diffused and dissolved to form Zr solute atoms under the high-temperature environment of electric arc.
Preferably, the Mg-Zr intermediate alloy pretreatment method for improving the magnesium alloy refining effect comprises the following specific steps:
a1, polishing the upper surface and the lower surface of the Mg-Zr intermediate alloy plate to be smooth, and fastening the Mg-Zr intermediate alloy plate on a copper seat with a water cooling device;
a2, carrying out multi-pass wire filling processing on the Mg-Zr intermediate alloy plate by using high-frequency pulse alternating current TIG welding under the state that a water cooling device of a copper seat is opened, so that large-size Zr clusters are dispersed and simultaneously diffused and dissolved under the high-temperature and high-frequency disturbance of an electric arc to form small-size Zr particles and partial solute Zr, wherein the solute Zr is fixedly dissolved in an Mg matrix under the subsequent chilling condition;
and A3, calculating new nominal components of the intermediate alloy after welding according to the proportion of the filled welding wire and the intermediate alloy, and polishing away the weld scale on the surface of the Mg-Zr intermediate alloy for later use.
In the prior art, large-size Zr particles in the Mg-Zr intermediate alloy are crushed into small-size Zr particles mainly through pretreatment processes such as large plastic deformation and the like so as to improve the refining effect of the small-size Zr particles. In contrast, the method adopts high-frequency pulse alternating current electric arc to carry out wire filling remelting on the Mg-Zr intermediate alloy, and realizes the conversion from particle Zr to solute Zr. Thus fundamentally avoiding the problem of sedimentation of large-size Zr particles in the Mg-Zr intermediate alloy due to high density in the smelting process; meanwhile, because the refining effect of the solute Zr on the magnesium alloy is stronger than that of the particle Zr, the pretreatment process improves the refining effect of the Mg-Zr intermediate alloy by improving the proportion of the solute Zr in the Mg-Zr intermediate alloy. Specifically, firstly, the pulse alternating current arc with high-frequency vibration has strong vibration effect on a molten pool in the welding process, so that large-size Zr particles agglomerated in the Mg-Zr intermediate alloy are dispersed and crushed firstly. Secondly, the high temperature generated by the electric arc is far higher than the melting temperature of the conventional magnesium alloy, and the dispersed small-size Zr particles are dissolved and diffused at high temperature to become solute Zr in a liquid phase. And by matching with pure magnesium welding wire filling, the proportion of magnesium in molten pool liquid metal can be increased, and more Zr is promoted to be dissolved into magnesium melt. And finally, rapidly solidifying the metal melt in the molten pool on a copper mould base with water cooling, so that solute atoms Zr in a liquid state are dissolved into the alpha-Mg matrix and are retained in the form of dissolved atoms. Therefore, the method can better promote the transformation of large-size Zr particles in the Mg-Zr intermediate alloy to the solute Zr, not only improves the refining effect of the Mg-Zr intermediate alloy on the magnesium alloy, but also can effectively avoid the fading effect generated by the refining effect of the Mg-Zr intermediate alloy.
Preferably, the mass fraction of Zr contained in the Mg-Zr intermediate alloy sheet is 10 to 30 percent, and the Mg-Zr intermediate alloy sheet is in an as-cast state or an extruded state.
Preferably, the wire filling material adopted by the wire filling processing is a cast-state or extruded-state pure magnesium welding wire, the diameter of the wire filling material is 2-6 mm, and the total amount of the wire filling is 1-50% of the mass of the Mg-Zr intermediate alloy plate to be pretreated. Pure magnesium is used as a wire filling material, so that the proportion of magnesium in liquid metal in a molten pool can be increased, and the Zr can be promoted to diffuse into a magnesium melt.
Preferably, in the step a1, the copper seat is made of copper or a copper alloy. The copper or the copper alloy has better heat-conducting property, can quickly take away the heat in the molten pool, and improves the cooling speed of the molten pool after welding.
Preferably, in the step a2, the welding current waveform adopted in the high-frequency pulse alternating current TIG welding is one of a square wave, a sine wave, a triangular wave and a sawtooth wave, the welding pulse frequency is 1000 to 20000Hz, and the welding alternating current frequency is 10 to 100 Hz. The high-frequency pulse alternating current arc can generate strong oscillation effect on a molten pool, and is favorable for promoting the large-size Zr agglomerate grains in the Mg-Zr intermediate alloy to be dispersed into small-size Zr grains.
Preferably, in the step a2, a welding base current and a welding peak current used in the high-frequency pulse alternating current TIG welding are each 50 to 250A, and the welding base current is 10 to 30A smaller than the welding peak current.
The invention also provides the Mg-Zr intermediate alloy which is obtained by the pretreatment method and can improve the magnesium alloy refining effect.
The invention also provides application of the Mg-Zr intermediate alloy which is obtained by the pretreatment method and can improve the magnesium alloy refining effect in magnesium alloy, and the application comprises the steps of immersing the Mg-Zr intermediate alloy obtained after pretreatment in magnesium liquid, and obtaining the magnesium alloy after grain refinement through conventional magnesium alloy smelting and pouring processes.
Preferably, the consumption of the Mg-Zr intermediate alloy obtained after the pretreatment is 1 to 10 percent of the mass of the magnesium liquid.
Compared with the prior art, the invention has the following beneficial effects:
1. the method utilizes the disturbance effect of the high-frequency alternating current arc on the molten pool to disperse Zr particles in the Mg-Zr intermediate alloy in a liquid environment, and simultaneously, the high temperature of the arc promotes the dispersed Zr particles to be continuously dissolved and diffused to the liquid phase of the molten pool. The invention not only realizes the conversion from large-particle Zr to small-particle Zr, but also realizes the conversion from small-particle Zr to solute atom Zr.
2. The pure magnesium welding wire improves the content of the alpha-Mg phase of the master alloy matrix, and more Zr solid solution atoms can be contained by more matrix content. After the electric arc is extinguished, the chilling effect of the water-cooling copper seat quickly dissolves a large amount of solute Zr dissolved in the molten pool into the matrix. The volume fraction of large-size Zr particles is reduced, and the content of solute Zr is increased, so that the pretreatment method can effectively improve the refining effect of the master alloy and prolong the refining decay time.
3. The invention only relates to a common TIG welding machine, and large-scale equipment such as a large-tonnage friction stir processing machine tool and the like is not needed. Meanwhile, the invention has short process flow, can be manually operated, and is flexible and convenient.
Drawings
Other features, objects and advantages of the invention will become more apparent upon reading of the detailed description of non-limiting embodiments with reference to the following drawings:
FIG. 1 is an operational view of a pretreatment method of an Mg-Zr intermediate alloy for improving the magnesium alloy fining effect according to the present invention;
in the figure, 1 is a pure magnesium welding wire, 2 is a high-frequency pulse alternating current TIG welding gun, 3 is a welding seam, 4 is a Mg-Zr intermediate alloy plate, 5 is a copper seat, and 6 is a cooling water pipeline.
Detailed Description
The present invention will be described in detail with reference to specific examples. The following examples will assist those skilled in the art in further understanding the invention, but are not intended to limit the invention in any way. It should be noted that it would be obvious to those skilled in the art that various changes and modifications can be made without departing from the spirit of the invention. All falling within the scope of the present invention.
It should be noted that, although the ingots of the conventional Mg-30 wt% Zr master alloys were used in examples 1 to 4, they were not the same ingot or different in the cutting position, and thus the distribution of Zr particles was not uniform.
Example 1
The experiment was carried out in two groups, taking the example of melting Mg-3 wt% Y-0.5 wt% Zr-Mg alloy.
Pretreatment of Mg-Zr intermediate alloy
A sheet is cut from a common Mg-30 wt% Zr intermediate alloy ingot, and Table 1 shows the particle size distribution of Zr particles in the Mg-Zr intermediate alloy counted by preparing metallographic samples, so that the particle size of the Zr particles in the Mg-Zr intermediate alloy before pretreatment is mainly concentrated in the range of 5-7 mu m.
TABLE 1 particle size distribution of Zr particles before pretreatment of Mg-Zr master alloy in example 1
| Particle size (. mu.m) | ＜1 | 1～3 | 3～5 | 5～7 | 7～9 | ＞9 |
| Ratio (%) | 7.9 | 14.5 | 17.7 | 25.4 | 18.9 | 15.6 |
Polishing the upper and lower surfaces of the cut Mg-Zr intermediate alloy plate to be in a smooth state by using abrasive paper, and fastening the Mg-Zr intermediate alloy plate on a copper seat (made of copper) with a water cooling device;
referring to fig. 1, a high-frequency pulse alternating current TIG welding gun 2 is used for carrying out multi-pass welding on a pure magnesium welding wire 1 filled in an Mg-Zr intermediate alloy plate 4 in a state that a water cooling device (specifically comprising a cooling water pipeline 6) of a copper seat 5 is opened, wherein the pure magnesium welding wire 1 is an extruded pure magnesium wire with the diameter of 2 mm. The total mass of the wire filling is 10 percent of the mass of the Mg-Zr intermediate alloy to be pretreated. The adopted current waveform is square wave, the pulse frequency is 1000Hz, and the alternating current frequency is 10 Hz. The base welding current was 50A and the peak current was 60A. And finally forming a welding seam 3 after the pretreatment is finished. Table 2 shows the particle size distribution of Zr particles in the pretreated Mg-Zr intermediate alloy counted by preparing metallographic samples, which shows that the particle size of the Zr particles in the pretreated Mg-Zr intermediate alloy is obviously reduced, the particle size is mainly concentrated at 1-3 mu m, and the number of the Zr particles on the matrix is obviously reduced, which indicates that part of Zr particles is converted into solute Zr.
TABLE 2 particle size distribution of Zr particles after pretreatment of Mg-Zr master alloy in example 1
| Particle size (. mu.m) | ＜1 | 1～3 | 3～5 | 5～7 | 7～9 | ＞9 |
| Ratio (%) | 18.9 | 29.6 | 17.6 | 16.4 | 12.2 | 5.3 |
And then calculating new nominal components of the welded intermediate alloy according to the proportion of the filled welding wires and the intermediate alloy, and polishing away the weld scale on the surface of the Mg-Zr intermediate alloy for later use.
Secondly, smelting and pouring Mg-3 wt% Y-0.5 wt% Zr magnesium alloy
In the first group of smelting experiments, pure magnesium ingots, Mg-25 wt% Y and Mg-Zr intermediate alloy ingots pretreated by the steps are prepared in advance according to the Mg-3 wt% Y-0.5 wt% Zr component according to a certain proportion.
Melting a pure magnesium ingot at the heating temperature of 680 ℃, then increasing the temperature of the melt to 730 ℃, adding an Mg-Y intermediate alloy ingot, increasing the temperature of the melt to 760 ℃ after the intermediate alloy ingot is melted, adding a pretreated Mg-Zr intermediate alloy accounting for 1 percent of the mass of magnesium liquid, standing and preserving heat for 30min after Zr is added. And (3) reducing the temperature of the melt to 740 ℃, refining for 10min, and controlling the casting temperature of the magnesium liquid to be 720 ℃. Through metallographic phase grain size statistical analysis, the grain size of the Mg-3 wt% Y-0.5 wt% Zr alloy refined by using the pretreated Mg-Zr intermediate alloy is 60-70 mu m.
The smelting and pouring conditions of the second set of experiment are consistent with those of the first set of experiment, only the pretreated Mg-Zr intermediate alloy used in the first set of experiment is changed into the common Mg-30 wt% Zr intermediate alloy, and through metallographic phase grain size statistical analysis, the grain size of the Mg-3 wt% Y-0.5 wt% Zr alloy prepared by the second set of smelting experiment is 70-80 μm.
The comparison of the two groups of experimental results shows that the method can effectively improve the grain refining effect of the Mg-Zr intermediate alloy on the magnesium alloy.
Example 2
The experiment was carried out in two groups, taking the example of melting Mg-3 wt% Gd-0.5 wt% Zr-Mg alloy.
Pretreatment of Mg-Zr intermediate alloy
A sheet was cut from a common Mg-30 wt.% Zr master alloy ingot. Table 3 shows the statistical distribution of Zr particles in the Mg-Zr intermediate alloy by preparing metallographic samples, and it can be seen that the Zr particles in the Mg-Zr intermediate alloy before pretreatment are mainly concentrated in the particle size of 5-7 μm.
TABLE 3 particle size distribution of Zr particles before pretreatment of Mg-Zr master alloy in example 2
Polishing the upper surface and the lower surface of the cut Mg-Zr intermediate alloy plate to be in a smooth state by using abrasive paper, and fastening the Mg-Zr intermediate alloy plate on a copper seat with a water cooling device;
referring to fig. 1, a high-frequency pulse alternating current TIG welding gun 2 is used for carrying out multi-pass welding on a pure magnesium wire 1 filled in a Mg-Zr intermediate alloy plate 4 under the state that a water cooling system 6 of a copper seat 5 is opened, and a welding wire is an extruded pure magnesium wire with the diameter of 4 mm. The total mass of the wire filling is 30 percent of the mass of the Mg-Zr intermediate alloy to be pretreated. The current waveform is a sine wave, the pulse frequency is 10000Hz, and the alternating current frequency is 50 Hz. The base welding current was 140A and the peak current was 160A. And finally forming a welding seam 3 after the pretreatment is finished. Table 4 shows the statistical distribution of Zr particles in the pretreated Mg-Zr intermediate alloy by preparing metallographic samples, which shows that the Zr particles in the pretreated Mg-Zr intermediate alloy are significantly reduced in particle size, the particle size is mainly concentrated in 1-3 μm, and the number of the Zr particles on the substrate is significantly reduced, indicating that some Zr particles are converted into solute Zr.
TABLE 4 particle size distribution of Zr particles after pretreatment of Mg-Zr master alloy in example 2
| Particle size (. mu.m) | ＜1 | 1～3 | 3～5 | 5～7 | 7～9 | ＞9 |
| Ratio (%) | 16.9 | 32.2 | 18.8 | 15.4 | 11.3 | 5.4 |
And then calculating new nominal components of the intermediate alloy after welding according to the proportion of the filled welding wire and the intermediate alloy, and polishing away the weld scale on the surface of the Mg-Zr intermediate alloy for later use.
Secondly, smelting and pouring Mg-3 wt% Gd-0.5 wt% Zr magnesium alloy
In the first group of smelting experiments, pure magnesium ingots, Mg-25 wt% of Gd and pretreated Mg-Zr intermediate alloy ingots are prepared in advance according to a certain proportion according to the components of Mg-3 wt% of Gd-0.5 wt% of Zr.
Melting a pure magnesium ingot at a heating temperature of 680 ℃, then increasing the temperature of the melt to 730 ℃, adding an Mg-Gd intermediate alloy ingot, increasing the temperature of the melt to 760 ℃ after the intermediate alloy ingot is melted, adding a pretreated Mg-Zr intermediate alloy accounting for 3% of the mass of magnesium liquid, standing and preserving heat for 30min after Zr addition is finished. And (3) reducing the temperature of the melt to 740 ℃, refining for 10min, and controlling the casting temperature of the magnesium liquid to be 720 ℃. Through metallographic phase grain size statistical analysis, the grain size of the Mg-3 wt% Gd-0.5 wt% Zr alloy refined by the pretreated Mg-Zr intermediate alloy is 60-70 mu m.
The smelting and pouring conditions of the second set of experiment are consistent with those of the first set of experiment, only the pretreated Mg-Zr intermediate alloy used in the first set of experiment is changed into the common Mg-30 wt% Zr intermediate alloy, and through metallographic phase grain size statistical analysis, the grain size of the Mg-3 wt% Gd-0.5 wt% Zr alloy prepared by the second set of smelting experiment is 70-80 μm.
The comparison of the two groups of experimental results shows that the method can effectively improve the grain refining effect of the Mg-Zr intermediate alloy on the magnesium alloy.
Example 3
Experiments were conducted in two groups, taking the example of melting Mg-3 wt% Nd-0.5 wt% Zr-Mg alloy.
Pretreatment of Mg-Zr intermediate alloy
A sheet was cut from a common Mg-30 wt.% Zr master alloy ingot. Table 5 shows the statistical distribution of Zr particles in the Mg-Zr intermediate alloy by preparing metallographic samples, and it can be seen that the Zr particles in the Mg-Zr intermediate alloy before pretreatment are mainly concentrated in the particle size of 7-9 μm.
TABLE 5 particle size distribution of Zr particles before pretreatment of Mg-Zr master alloy in example 3
| Particle size (. mu.m) | ＜1 | 1～3 | 3～5 | 5～7 | 7～9 | ＞9 |
| Ratio (%) | 6.9 | 6.2 | 18.7 | 22.9 | 26.6 | 18.7 |
Polishing the upper surface and the lower surface of the cut Mg-Zr intermediate alloy plate to be in a smooth state by using abrasive paper, and fastening the Mg-Zr intermediate alloy plate on a copper seat with a water cooling device;
referring to fig. 1, a high-frequency pulse alternating current TIG welding gun 2 is used for carrying out multi-pass welding on a pure magnesium wire 1 filled in a Mg-Zr intermediate alloy plate 4 under the state that a water cooling system 6 of a copper seat 5 is opened, and a welding wire is an extruded pure magnesium wire with the diameter of 6 mm. The total mass of the wire filling is 50 percent of the mass of the Mg-Zr intermediate alloy to be pretreated. The current waveform is triangular wave, the pulse frequency is 20000Hz, and the alternating current frequency is 100 Hz. The base welding current was 220A and the peak current was 250A. And finally forming a welding seam 3 after the pretreatment is finished. Table 6 shows the statistical distribution of Zr particles in the pretreated Mg-Zr intermediate alloy by preparing metallographic samples, which shows that the Zr particles in the pretreated Mg-Zr intermediate alloy are significantly reduced in particle size, the particle size is mainly concentrated in 1-3 μm, and the number of Zr particles on the substrate is significantly reduced, indicating that some Zr particles are converted into solute Zr.
TABLE 6 particle size distribution of Zr particles after pretreatment of Mg-Zr master alloy in example 3
| Particle size (. mu.m) | ＜1 | 1～3 | 3～5 | 5～7 | 7～9 | ＞9 |
| Ratio (%) | 15.1 | 28.8 | 22.2 | 16.5 | 13.3 | 4.1 |
And then calculating new nominal components of the intermediate alloy after welding according to the proportion of the filled welding wire and the intermediate alloy, and polishing away the weld scale on the surface of the Mg-Zr intermediate alloy.
Secondly, smelting and pouring Mg-3 wt% Nd-0.5 wt% Zr-magnesium alloy
In the first group of smelting experiments, pure magnesium ingots, Mg-25 wt% of Nd and pretreated Mg-Zr intermediate alloy ingots are prepared in advance according to a certain proportion according to the components of Mg-3 wt% of Nd and 0.5 wt% of Zr.
Melting a pure magnesium ingot at a heating temperature of 680 ℃, then increasing the temperature of the melt to 730 ℃, adding an Mg-Nd intermediate alloy ingot, increasing the temperature of the melt to 760 ℃ after the intermediate alloy ingot is melted, adding a pretreated Mg-Zr intermediate alloy accounting for 6% of the mass of magnesium liquid, standing and preserving heat for 30min after Zr is added. And (3) reducing the temperature of the melt to 740 ℃, refining for 10min, and controlling the casting temperature of the magnesium liquid to be 720 ℃. Through metallographic phase grain size statistical analysis, the grain size of the Mg-3 wt% Nd-0.5 wt% Zr alloy refined by using the pretreated Mg-Zr intermediate alloy is 50-60 mu m.
The smelting and pouring conditions of the second set of experiments are consistent with those of the first set of experiments, only the pretreated Mg-Zr intermediate alloy used in the first set of experiments is changed into a common Mg-30 wt% Zr intermediate alloy, and through metallographic grain size statistical analysis, the grain size of the Mg-3 wt% Nd-0.5 wt% Zr alloy prepared by the second set of smelting experiments is 80-90 μm.
The comparison of the two groups of experimental results shows that the method can effectively improve the grain refining effect of the Mg-Zr intermediate alloy on the magnesium alloy.
Example 4
The experiment was carried out in two groups, taking the example of melting Mg-6 wt% Zn-0.5 wt% Zr-Mg alloy.
Pretreatment of Mg-Zr intermediate alloy
A sheet was cut from a common Mg-30 wt.% Zr master alloy ingot. Table 7 shows the statistical distribution of Zr particles in the Mg-Zr intermediate alloy by preparing metallographic samples, and it can be seen that the Zr particles in the Mg-Zr intermediate alloy before pretreatment are mainly concentrated in the particle size of 5-7 μm.
TABLE 7 particle size distribution of Zr particles before pretreatment of Mg-Zr master alloy in example 4
| Particle size (. mu.m) | ＜1 | 1～3 | 3～5 | 5～7 | 7～9 | ＞9 |
| Ratio (%) | 5.4 | 8.8 | 17.4 | 27.7 | 21.3 | 19.4 |
Polishing the upper surface and the lower surface of the cut Mg-Zr intermediate alloy plate to be in a smooth state by using abrasive paper, and fastening the Mg-Zr intermediate alloy plate on a copper seat with a water cooling device;
referring to fig. 1, a high-frequency pulse alternating current TIG welding gun 2 is used for carrying out multi-pass welding on a pure magnesium wire 1 filled in a Mg-Zr intermediate alloy plate 4 under the state that a water cooling system 6 of a copper seat 5 is opened, and a welding wire is an extruded pure magnesium wire with the diameter of 6 mm. The total mass of the wire filling is 50 percent of the mass of the Mg-Zr intermediate alloy to be pretreated. The current waveform is sine wave, the pulse frequency is 20000Hz, and the alternating current frequency is 100 Hz. The base welding current was 240A and the peak current was 250A. And finally forming a welding seam 3 after the pretreatment is finished. Table 8 shows the statistical distribution of Zr particles in the pretreated Mg-Zr intermediate alloy by preparing metallographic samples, which shows that the Zr particles in the pretreated Mg-Zr intermediate alloy are significantly reduced in size, mainly concentrated at 1-3 μm in size, and that the Zr particles on the substrate are significantly reduced in number, indicating that some Zr particles are converted into solute Zr.
TABLE 8 particle size distribution of Zr particles after pretreatment of Mg-Zr master alloy in example 4
| Particle size (. mu.m) | ＜1 | 1～3 | 3～5 | 5～7 | 7～9 | ＞9 |
| Ratio (%) | 17.4 | 26.6 | 23.7 | 18.4 | 12.1 | 1.8 |
And then calculating new nominal components of the welded intermediate alloy according to the proportion of the filled welding wires and the intermediate alloy, and polishing away the weld scale on the surface of the Mg-Zr intermediate alloy.
Secondly, smelting and pouring Mg-6 wt% Zn-0.5 wt% Zr magnesium alloy
In the first group of smelting experiments, pure magnesium ingots, Mg-30 wt% of Zn and pretreated Mg-Zr intermediate alloy ingots are prepared in advance according to a certain proportion according to the components of Mg-6 wt% of Zn and 0.5 wt% of Zr.
Melting a pure magnesium ingot at a heating temperature of 680 ℃, then increasing the temperature of the melt to 720 ℃, adding an Mg-Zn intermediate alloy ingot, increasing the temperature of the melt to 760 ℃ after the intermediate alloy ingot is melted, adding a pretreated Mg-Zr intermediate alloy accounting for 10% of the mass of magnesium liquid, standing and preserving heat for 30min after Zr is added. And (3) reducing the temperature of the melt to 740 ℃, refining for 10min, and controlling the casting temperature of the magnesium liquid to be 720 ℃. Through metallographic phase grain size statistical analysis, the grain size of the Mg-6 wt% Zn-0.5 wt% Zr alloy refined by using the pretreated Mg-Zr intermediate alloy is 50-60 mu m.
The smelting and pouring conditions of the second set of experiments are consistent with those of the first set of experiments, only the pretreated Mg-Zr intermediate alloy used in the first set of experiments is changed into a common Mg-30 wt% Zr intermediate alloy, and through metallographic grain size statistical analysis, the grain size of the Mg-6 wt% Zn-0.5 wt% Zr alloy prepared by the second set of smelting experiments is 90-100 mu m.
The comparison of the two groups of experimental results shows that the method can effectively improve the grain refining effect of the Mg-Zr intermediate alloy on the magnesium alloy.
Example 5
The experiment was carried out in two groups, taking the example of melting Mg-3 wt% Y-0.5 wt% Zr-Mg alloy.
Pretreatment of Mg-Zr intermediate alloy
A sheet was cut from a common Mg-10 wt.% Zr master alloy ingot. Table 9 shows the statistical distribution of Zr particles in the Mg-Zr intermediate alloy by preparing metallographic samples, which indicates that the Zr particles in the Mg-Zr intermediate alloy before pretreatment are mainly concentrated in the particle size range of 3-5 μm.
TABLE 9 particle size distribution of Zr particles before pretreatment of Mg-Zr master alloy in example 5
| Particle size (. mu.m) | ＜1 | 1～3 | 3～5 | 5～7 | 7～9 | ＞9 |
| Ratio (%) | 10.8 | 16.2 | 22.6 | 18.4 | 17.6 | 14.4 |
Polishing the upper surface and the lower surface of the cut Mg-Zr intermediate alloy plate to be in a smooth state by using abrasive paper, and fastening the Mg-Zr intermediate alloy plate on a copper seat with a water cooling device;
referring to fig. 1, a high-frequency pulse alternating current TIG welding gun 2 is used for carrying out multi-pass welding on a pure magnesium wire 1 filled in a Mg-Zr intermediate alloy plate 4 under the state that a water cooling system 6 of a copper seat 5 is opened, and a welding wire is an extruded pure magnesium wire with the diameter of 6 mm. The total mass of the wire filling is 50 percent of the mass of the Mg-Zr intermediate alloy to be pretreated. The current waveform is triangular wave, the pulse frequency is 20000Hz, and the alternating current frequency is 100 Hz. The base welding current was 220A and the peak current was 250A. And finally forming a welding seam 3 after the pretreatment is finished. Table 10 shows the statistical distribution of Zr particles in the pretreated Mg-Zr intermediate alloy by preparing metallographic samples, which shows that the Zr particles in the pretreated Mg-Zr intermediate alloy are significantly reduced in size, mainly concentrated at 1-3 μm in size, and that the Zr particles on the substrate are significantly reduced in number, indicating that some Zr particles are converted into solute Zr.
TABLE 10 particle size distribution of Zr particles after pretreatment of Mg-Zr master alloy in example 5
| Particle size (. mu.m) | ＜1 | 1～3 | 3～5 | 5～7 | 7～9 | ＞9 |
| Ratio (%) | 22.9 | 28.4 | 21.7 | 11.5 | 8.8 | 6.7 |
And then calculating new nominal components of the welded intermediate alloy according to the proportion of the filled welding wires and the intermediate alloy, and polishing away the weld scale on the surface of the Mg-Zr intermediate alloy.
Secondly, smelting and pouring Mg-3 wt% Y-0.5 wt% Zr magnesium alloy
In the first group of smelting experiments, pure magnesium ingots, Mg-25 wt% Y and Mg-Zr intermediate alloy ingots pretreated by the steps are prepared in advance according to the Mg-3 wt% Y-0.5 wt% Zr component according to a certain proportion.
Melting a pure magnesium ingot at the heating temperature of 680 ℃, then increasing the temperature of the melt to 730 ℃, adding an Mg-Y intermediate alloy ingot, increasing the temperature of the melt to 760 ℃ after the intermediate alloy ingot is melted, adding a pretreated Mg-Zr intermediate alloy accounting for 10% of the mass of magnesium liquid, standing and preserving heat for 30min after Zr is added. And (3) reducing the temperature of the melt to 740 ℃, refining for 10min, and controlling the casting temperature of the magnesium liquid to be 720 ℃. Through metallographic phase grain size statistical analysis, the grain size of the Mg-3 wt% Y-0.5 wt% Zr alloy refined by using the pretreated Mg-Zr intermediate alloy is 50-60 mu m.
The smelting and pouring conditions of the second set of experiment are consistent with those of the first set of experiment, only the pretreated Mg-Zr intermediate alloy used in the first set of experiment is changed into the common Mg-10 wt% Zr intermediate alloy, and through metallographic phase grain size statistical analysis, the grain size of the Mg-3 wt% Y-0.5 wt% Zr alloy prepared by the second set of smelting experiment is 60-70 μm.
The comparison of the two groups of experimental results shows that the method can effectively improve the grain refining effect of the Mg-Zr intermediate alloy on the magnesium alloy.
Example 6
The experiment was carried out in two groups, taking the example of melting Mg-3 wt% Y-0.5 wt% Zr-Mg alloy.
Pretreatment of Mg-Zr intermediate alloy
A sheet was cut from a common Mg-20 wt.% Zr master alloy ingot. Table 11 shows the statistical distribution of Zr particles in the Mg-Zr intermediate alloy by preparing metallographic samples, and it can be seen that the Zr particles in the Mg-Zr intermediate alloy before pretreatment are mainly concentrated in 3-5 μm.
TABLE 11 particle size distribution of Zr particles before pretreatment of Mg-Zr master alloy in example 6
| Particle size (. mu.m) | ＜1 | 1～3 | 3～5 | 5～7 | 7～9 | ＞9 |
| Ratio (%) | 4.1 | 17.2 | 26.4 | 20.7 | 18.5 | 13.1 |
Polishing the upper surface and the lower surface of the cut Mg-Zr intermediate alloy plate to be in a smooth state by using abrasive paper, and fastening the Mg-Zr intermediate alloy plate on a copper seat with a water cooling device;
referring to fig. 1, a high-frequency pulse alternating current TIG welding gun 2 is used for carrying out multi-pass welding on a pure magnesium wire 1 filled in a Mg-Zr intermediate alloy plate 4 under the state that a water cooling system 6 of a copper seat 5 is opened, and a welding wire is an extruded pure magnesium wire with the diameter of 6 mm. The total mass of the wire filling is 50 percent of the mass of the Mg-Zr intermediate alloy to be pretreated. The current waveform is sine wave, the pulse frequency is 20000Hz, and the alternating current frequency is 100 Hz. The base welding current was 240A and the peak current was 250A. And finally forming a welding seam 3 after the pretreatment is finished. Table 12 shows the statistical distribution of Zr particles in the pretreated Mg-Zr intermediate alloy by preparing metallographic samples, which shows that the Zr particles in the pretreated Mg-Zr intermediate alloy are significantly reduced in size, mainly concentrated in 1-3 μm, and the number of Zr particles on the substrate is significantly reduced, indicating that some Zr particles are converted into solute Zr.
TABLE 12 particle size distribution of Zr particles after pretreatment of Mg-Zr master alloy in example 6
| Particle size (. mu.m) | ＜1 | 1～3 | 3～5 | 5～7 | 7～9 | ＞9 |
| Ratio (%) | 18.9 | 21.1 | 24.5 | 13.6 | 11.2 | 10.7 |
And then calculating new nominal components of the welded intermediate alloy according to the proportion of the filled welding wires and the intermediate alloy, and polishing away the weld scale on the surface of the Mg-Zr intermediate alloy.
Secondly, smelting and pouring Mg-3 wt% Y-0.5 wt% Zr magnesium alloy
In the first group of smelting experiments, pure magnesium ingots, Mg-25 wt% Y and Mg-Zr intermediate alloy ingots pretreated by the steps are prepared in advance according to the Mg-3 wt% Y-0.5 wt% Zr component according to a certain proportion.
Melting a pure magnesium ingot at the heating temperature of 680 ℃, then increasing the temperature of the melt to 730 ℃, adding an Mg-Y intermediate alloy ingot, increasing the temperature of the melt to 760 ℃ after the intermediate alloy ingot is melted, adding a pretreated Mg-Zr intermediate alloy accounting for 5% of the mass of magnesium liquid, standing and preserving heat for 30min after Zr is added. And (3) reducing the temperature of the melt to 740 ℃, refining for 10min, and controlling the casting temperature of the magnesium liquid to be 720 ℃. Through metallographic phase grain size statistical analysis, the grain size of the Mg-3 wt% Y-0.5 wt% Zr alloy refined by using the pretreated Mg-Zr intermediate alloy is 60-70 mu m.
The smelting and pouring conditions of the second set of experiment are consistent with those of the first set of experiment, only the pretreated Mg-Zr intermediate alloy used in the first set of experiment is changed into the common Mg-10 wt% Zr intermediate alloy, and through metallographic phase grain size statistical analysis, the grain size of the Mg-3 wt% Y-0.5 wt% Zr alloy prepared by the second set of smelting experiment is 70-80 μm.
The comparison of the two groups of experimental results shows that the method can effectively improve the grain refining effect of the Mg-Zr intermediate alloy on the magnesium alloy.
Comparative example 1
This comparative example is substantially the same as the pretreatment method of the Mg-Zr intermediate alloy of example 1, and the grain size of Zr particles in the Mg-Zr intermediate alloy before the pretreatment used is the same as that of example 1 except that: the pulse frequency used was 500 Hz.
Table 13 shows the distribution of Zr particles in the pretreated Mg-Zr intermediate alloy counted by preparing metallographic samples, which indicates that the Zr particles in the pretreated Mg-Zr intermediate alloy have no significant refinement.
TABLE 13 particle size distribution of Zr particles after pretreatment of Mg-Zr master alloy in comparative example 1
| Particle size (. mu.m) | ＜1 | 1～3 | 3～5 | 5～7 | 7～9 | ＞9 |
| Ratio (%) | 8.6 | 15.2 | 17.9 | 24.7 | 18.1 | 15.5 |
Comparative example 2
This comparative example is substantially the same as the pretreatment method of the Mg-Zr intermediate alloy of example 1, and the grain size of Zr particles in the Mg-Zr intermediate alloy before the pretreatment used is the same as that of example 1 except that: the pre-treatment welding process was not performed on a copper base with water cooling, but on a conventional Q345 steel backing plate.
Table 14 shows the statistical distribution of Zr particles in the pretreated Mg-Zr intermediate alloy by preparing metallographic samples, which indicates that the Zr particles in the pretreated Mg-Zr intermediate alloy have insignificant particle size refinement.
TABLE 14 particle size distribution of Zr particles after pretreatment of Mg-Zr master alloy in comparative example 2
| Particle size (. mu.m) | ＜1 | 1～3 | 3～5 | 5～7 | 7～9 | ＞9 |
| Ratio (%) | 9.2 | 16.5 | 18.4 | 23.6 | 17.7 | 14.6 |
The foregoing description of specific embodiments of the present invention has been presented. It is to be understood that the present invention is not limited to the specific embodiments described above, and that various changes or modifications may be made by one skilled in the art within the scope of the appended claims without departing from the spirit of the invention. The embodiments and features of the embodiments of the present application may be combined with each other arbitrarily without conflict.
Claims (8)
1. A Mg-Zr intermediate alloy pretreatment method for improving the magnesium alloy refining effect is characterized by comprising the step of carrying out multi-pass wire filling processing on a Mg-Zr intermediate alloy plate by using high-frequency pulse alternating current TIG welding;
the wire filling material adopted by the wire filling processing is a cast-state or extruded-state pure magnesium welding wire, the diameter of the wire filling material is 2-6 mm, and the total amount of the wire filling is 1-50% of the mass of the Mg-Zr intermediate alloy plate to be pretreated;
the pretreatment method comprises the following specific steps:
a1, polishing the upper surface and the lower surface of the Mg-Zr intermediate alloy plate to be smooth, and fastening the Mg-Zr intermediate alloy plate on a copper seat with a water cooling device;
a2, performing multi-pass wire filling processing on the Mg-Zr intermediate alloy plate by using high-frequency pulse alternating current TIG welding in a state that a water cooling device of the copper seat is opened;
a3, calculating new nominal composition of the intermediate alloy after welding according to the proportion of the filled welding wire and the intermediate alloy, and polishing away the weld scale on the surface of the Mg-Zr intermediate alloy for later use.
2. The pretreatment method of an Mg-Zr intermediate alloy for improving the refinement effect of magnesium alloy according to claim 1, characterized in that the mass fraction of Zr contained in the Mg-Zr intermediate alloy sheet is 10% to 30%, and the Mg-Zr intermediate alloy sheet is in an as-cast state or an extruded state.
3. The pretreatment method of Mg-Zr intermediate alloy for improving the refinement effect of magnesium alloy according to claim 1, wherein the copper base used in the step A1 is copper or copper alloy.
4. The pretreatment method for Mg-Zr intermediate alloy for improving magnesium alloy refining effect according to claim 1, characterized in that in the step A2, the welding current waveform adopted by the high-frequency pulse alternating current TIG welding is one of square wave, sine wave, triangular wave or sawtooth wave, the welding pulse frequency is 1000 to 20000Hz, and the welding alternating current frequency is 10 to 100 Hz.
5. The pretreatment method for an Mg-Zr intermediate alloy for improving the refinement effect of a magnesium alloy according to claim 1, characterized in that in the step A2, the welding base current and the welding peak current used in the high-frequency pulse alternating current TIG welding are 50 to 250A each, and the welding base current is 10 to 30A smaller than the welding peak current.
6. An Mg-Zr intermediate alloy capable of improving the refining effect of magnesium alloy, obtained by the pretreatment method according to any one of claims 1 to 5.
7. The application of the Mg-Zr intermediate alloy for improving the magnesium alloy refining effect in the magnesium alloy according to claim 6 is characterized by comprising the steps of immersing the Mg-Zr intermediate alloy obtained after pretreatment in magnesium liquid, and obtaining the magnesium alloy after grain refinement through magnesium alloy smelting and pouring processes.
8. The use according to claim 7, wherein the amount of the Mg-Zr intermediate alloy obtained after the pretreatment is 1-10% of the mass of the molten magnesium.
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