CN109266889B - Composite refining method of zirconium-containing magnesium alloy - Google Patents
Composite refining method of zirconium-containing magnesium alloy Download PDFInfo
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- C22C1/03—Making non-ferrous alloys by melting using master alloys
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Abstract
The invention discloses a composite refining method of zirconium-containing magnesium alloy, which comprises the following steps: a. adding a magnesium ingot into the first heating device to melt the magnesium ingot into a molten magnesium melt; b. adding alloy element ingots into the molten magnesium melt to obtain an intermediate magnesium melt; c. adding magnesium-zirconium intermediate alloy into the alloy intermediate melt, and continuously stirring by using a stirring device to obtain an alloy melt; d. removing floating slag on the surface of the alloy melt; e. adding a flux for refining into the alloy melt; f. adding refining gas into the alloy solution through a gas conveying device; g. the temperature of the alloy melt is reduced to its casting temperature. Through respectively carrying out alloying on the zirconium-free alloy and the magnesium-zirconium intermediate alloy, the zirconium element particles which have been deposited are returned to the alloy intermediate melt for remelting, so that the solubility of zirconium in the alloy intermediate melt can be improved, the yield of zirconium is improved, and the production cost is also reduced.
Description
Technical Field
The invention relates to the technical field of zirconium-containing magnesium alloy smelting, in particular to a composite refining method of a zirconium-containing magnesium alloy.
Background
To improve the magnesium alloyThe inclusions in the magnesium alloy are generally present in the grain boundary or matrix of the magnesium alloy structure in the form of particles, clusters or films, and can be classified into three types, namely non-metallic inclusions, metallic inclusions and gas according to the composition and structure, ① the non-metallic inclusions comprise oxynitride of magnesium (MgO, Mg)3N2) Metal halide (KCl, NaCl, CaCl)2、MgCl2Etc.), aluminum calcium based carbides (CaC, Al)4C3Etc.), magnesium aluminum based fluorides and magnesium based sulfides (MgSO)4、MgS、AlF3、MgF2) ② the metallic inclusions include α -Fe particles and Mn-Fe metal compounds (e.g., MnAl)4、Fe2(Si,B)、(Fe,Mn)3Si、Fe3(A1,Si)、MnAl6Or MnAl6、(Fe,Mn)5Si3、(Fe,Mn)3Si, etc.), Zr-Fe metal compounds (e.g. Zr)3Fe、ZrFe3、Zr2Fe、ZrFe2) Etc. ③ the gas is primarily hydrogen.
The family of alloys that include zircaloy includes magnesium-zinc-zirconium alloys, magnesium-rare earth-zinc-zirconium alloys, and magnesium-thorium based and magnesium-silver based zircaloys. Zirconium (Zr) is the most effective grain refiner of magnesium alloy materials, and currently, a magnesium-zirconium intermediate alloy is generally used in industry to add zirconium to achieve the purpose of grain refinement, so that the hot cracking tendency of the alloy is reduced, and the properties of the alloy, such as strength, plasticity, creep resistance, corrosion resistance and the like, are improved to meet the requirements of the aviation and aerospace industries. Compared with magnesium (Mg melting point 651 ℃, density 1.74 g/cm)3) The metal element zirconium has high melting point and high density (the melting point of Zr is 1855 ℃, and the density is 6.52 g/cm)3) The added zirconium is difficult to completely melt into the magnesium melt, and exists in the magnesium melt in both a dissolved state and an undissolved state. Therefore, in addition to the three common inclusions mentioned above, a new type of inclusion occurs during the smelting of the zircaloy alloy: undissolved zirconium particles.
During the smelting process of the zirconium-containing magnesium alloy, undissolved zirconium particles mainly cause the following two problems:
1. the zirconium yield is reduced. The undissolved zirconium particles have high density and are quickly settled to the bottom of the crucible, so that the zirconium yield is reduced. The inclusions are assumed to be spheres and only influenced by the resistance, buoyancy and gravity of the magnesium melt, and only move in the vertical direction in the sinking process, and the Reynolds coefficient Re of the movement of the inclusions in the standing process of the melt is less than 0.6. According to the calculation of Stokes' formula, in the process of smelting Mg-Nd-Zn-Zr, when the approximate sphere diameter of zirconium particles is 10 μm, the settling distance after standing for 10min is about 0.18m, and when the size of the inclusions is 50 μm, the settling distance after standing for 10min is about 4.41 m. In order to compensate for the loss of zirconium in the smelting process and obtain the target zirconium content, about 3 times of magnesium-zirconium intermediate alloy is generally added in the production, so that the production cost is greatly improved.
2. The zirconium grain refinement effect is impaired. The influence of zirconium particle sedimentation on grain refinement is embodied in two aspects, one is that the content of dissolved zirconium is reduced to influence the grain refinement, and the other is that undissolved zirconium influences the grain refinement, so that the performance of the zirconium-containing magnesium alloy is influenced.
Disclosure of Invention
The invention aims to solve the technical problem of providing a composite refining method of a zirconium-containing magnesium alloy, which has low production cost, high zirconium yield and good grain refinement effect.
The invention discloses a composite refining method of a zirconium-containing magnesium alloy, which is used for solving the technical problem and comprises the following steps:
a. adding a magnesium ingot into a first heating device, and melting the magnesium ingot into a molten magnesium melt by the first heating device;
b. stirring the molten magnesium melt by a stirring device, continuously heating by a first heating device to ensure that alloy element ingots are added into the molten magnesium melt when the temperature of the molten magnesium melt reaches 740-760 ℃, and continuously stirring by the stirring device for a certain time to obtain an intermediate magnesium melt;
c. in the process of stirring the intermediate magnesium melt by the stirring device, when the first heating device continues to heat the intermediate magnesium melt to 780-800 ℃, adding magnesium-zirconium intermediate alloy into the intermediate magnesium melt, and continuing to stir for a certain time by the stirring device to obtain alloy melt;
d. removing floating slag on the surface of the alloy melt;
e. reducing the temperature of the alloy melt to 750-760 ℃, adding a flux for refining into the alloy melt, and continuously stirring for a certain time by using a stirring device;
f. the temperature of the alloy melt is maintained between 750 ℃ and 760 ℃, and gas for refining is added into the alloy melt through a gas conveying device;
g. the temperature of the alloy melt is reduced to its casting temperature.
Further, in the step a, after the first heating device is electrified and preheated to 400-500 ℃, the magnesium ingot is added into the first heating device.
Further, agitating unit includes motor, reduction gear, connecting axle, agitator, and the agitator is axial impulse type agitator, and the output shaft of motor is connected with the reduction gear, and connecting axle one end is connected with the reduction gear, and the other end is connected with the agitator.
Further, the first heating device is internally provided with a sleeve or 4-6 baffles, and 4-6 baffles are evenly distributed on the inner surface of the first heating device.
Further, in the step b, a stirrer in the stirring device extends deeply into the molten magnesium melt for stirring, the stirrer is positioned at one third of the height of the molten magnesium melt, the alloy element ingot is preheated by the second heating device and then added into the molten magnesium melt, and the stirring time of the stirring device is 3-5min after the alloy element ingot is added into the molten magnesium melt.
Further, in the step c, preheating a magnesium-zirconium intermediate alloy by a third heating device, adding the preheated magnesium-zirconium intermediate alloy into the intermediate magnesium melt, adding the magnesium-zirconium intermediate alloy into the intermediate magnesium melt, then enabling a stirrer in a stirring device to go deep into one third of the height of the intermediate magnesium melt and stirring for 1-3min, then sinking the stirrer into the bottom of the intermediate magnesium melt and stirring for 1-3min, and finally, raising the stirrer to one third of the height of the intermediate magnesium melt and stirring for 1-3 min.
Further, in the step e, a refining flux RJ-5 is added into the alloy melt, and the stirring device continuously stirs for 10-15 min.
Further, gas conveying device includes gas tank, desicator, guide arm, rotatory nozzle, and the gas tank is connected with guide arm one end through the trachea, and the other end of guide arm is connected with rotatory nozzle, and the desicator setting is on the trachea.
Further, in the step f, the refining gas is argon or/and nitrogen, and the refining gas is introduced for 5-10 min.
The invention has the beneficial effects that:
1. the zirconium alloying is independently carried out, and the magnesium-zirconium alloying temperature is increased to 780-800 ℃, so that the solubility of zirconium in the intermediate magnesium melt can be improved, the yield of zirconium is improved, and the production cost is reduced.
2. Stirring is carried out through a stirring device in the refining process, large-range axial and radial flow and small-area turbulence are formed in the molten magnesium melt, the intermediate magnesium melt and the alloy melt, heat transmission from the outer edge of each melt to the central part is enhanced, and element uniform mixing in each melt is promoted.
3. After the magnesium-zirconium intermediate alloy is added into the intermediate magnesium melt, a stirrer in a stirring device extends into one third of the height of the intermediate magnesium melt and is stirred for 1-3min, then the stirrer is sunk into the bottom of the intermediate magnesium melt and is stirred for 1-3min, and finally the stirrer is lifted to one third of the height of the intermediate magnesium melt and is stirred for 1-3min, so that zirconium element particles sinking to the bottom in the intermediate magnesium melt are re-melted in the intermediate magnesium melt, the zirconium yield is further improved, the grain refining effect is improved, and the production cost is reduced.
4. The composite refining technology of firstly flux refining, then gas refining and finally standing sedimentation is adopted, so that sinking impurities, floating impurities and gas are effectively removed, the produced zirconium-containing magnesium alloy has the advantages of less impurities, good purification effect and high purity of the zirconium-containing magnesium alloy.
Drawings
FIG. 1 is a schematic front view of a stirring device in a first heating device;
FIG. 2 is a schematic top view of the stirring device in the first heating device;
FIG. 3 is a schematic view of the gas delivery device being vented to the first heating means;
parts and numbering in the figures: the device comprises a first heating device 1, a baffle 2, a connecting shaft 3, a stirrer 4, a guide rod 5 and a rotary spray head 6.
Detailed Description
The invention will be further explained with reference to the drawings.
As shown in fig. 1, 2 and 3, the composite refining method of the zirconium-containing magnesium alloy of the present invention comprises the following steps:
a. adding a magnesium ingot into the first heating device 1, and melting the magnesium ingot into a molten magnesium melt by the first heating device 1;
b. stirring the molten magnesium melt by a stirring device, continuously heating by a first heating device 1 to ensure that alloy element ingots are added into the molten magnesium melt when the temperature of the molten magnesium melt reaches 740-760 ℃, and continuously stirring by the stirring device for a certain time to obtain an intermediate magnesium melt;
c. in the process of stirring the intermediate magnesium melt by the stirring device, when the temperature of the intermediate magnesium melt is increased to 780-800 ℃ by continuously heating the first heating device 1, adding magnesium-zirconium intermediate alloy into the intermediate magnesium melt, and continuously stirring for a certain time by the stirring device to obtain an alloy melt;
d. removing floating slag on the surface of the alloy melt;
e. reducing the temperature of the alloy melt to 750-760 ℃, adding a flux for refining into the alloy melt, and continuously stirring for a certain time by using a stirring device;
f. the temperature of the alloy melt is maintained between 750 ℃ and 760 ℃, and gas for refining is added into the alloy melt through a gas conveying device;
g. standing for 10min, further removing impurities by a gravity settling means, then cooling to a casting temperature, and carrying out subsequent operations of deslagging, liquid transferring, pouring and the like.
Specifically, in order to improve the heating efficiency in refining, the first heating device 1 may be placed in a heating furnace, and each melt (all the melts described above) in the first heating device 1 extracts energy from the heating furnace. In order to prevent a safety accident caused by water contained in the crucible, the first heating device 1 is electrically preheated to 400-.
In the step b, the first heating device 1 continues to heat to make the temperature of the molten magnesium melt reach 740-. In the alloying process, a stirrer 4 in the stirring device is deeply inserted into the molten magnesium melt for stirring, the stirrer 4 is positioned at one third of the height of the molten magnesium melt, the alloy element ingot is preheated by the second heating device and then added into the molten magnesium melt, and the stirring time of the stirring device is 3-5min after the alloy element ingot is added into the molten magnesium melt.
In the step c, preheating the magnesium-zirconium intermediate alloy by a third heating device, adding the preheated magnesium-zirconium intermediate alloy into the intermediate magnesium melt, adding the magnesium-zirconium intermediate alloy into the intermediate magnesium melt, then enabling a stirrer 4 in a stirring device to go deep into one third of the height of the intermediate magnesium melt and stirring for 1-3min, then enabling the stirrer 4 to be positioned at the bottom of the intermediate magnesium melt and stirring for 1-3min, and finally enabling the stirrer 4 to be positioned at one third of the height of the intermediate magnesium melt and stirring for 1-3 min.
In the step e, a refining flux of RJ-5 is added into the alloy melt, and the stirring device continuously stirs for 10-15 min.
In the step f, the refining gas is argon or/and nitrogen, and the refining gas is introduced for 5-10 min.
During the composite refining of Zr-Mg alloy, covering flux and protecting gas may be added to separate the melts from air, the flux for washing smelting tool may be RJ-1, the covering flux may be RJ-2, and the protecting gas may be CO2And 0.18% SF6。
The stirring device of the present invention functions as: mixing, dispersing, strengthening heat and mass transfer, uniformly suspending solid particles (refractory zirconium element particles) in each melt, accelerating chemical reaction and the like. The preferred structure of the stirring device of the invention is as follows: as shown in fig. 1 and 2, the stirring device includes a motor, a reducer, a connecting shaft 3, and a stirrer 4, the stirrer 4 is an axial propelling stirrer, an output shaft of the motor is connected to the reducer, one end of the connecting shaft 3 is connected to the reducer, the other end of the connecting shaft 3 is connected to the stirrer 4, the motor rotates to drive the reducer to rotate, the reducer rotates to drive the connecting shaft 3 to rotate, the connecting shaft 3 rotates to drive the stirrer 4 to rotate, and the molten magnesium, the intermediate magnesium, and the alloy melt are stirred by the axial propelling stirrer 4 in the stirring device during refining to form large-range axial and radial flows and small-range turbulence in the molten magnesium melt, so as to enhance heat transmission from the outer edge of each melt to the core, promote uniform mixing of elements in each melt, especially form axial macroscopic rotary flow for zirconium-containing magnesium alloy, promote the bottom of the first heating device 1, The melt at the middle part and the melt at the upper part are mutually fused to complete the uniform mixing and dispersion of the alloy elements. After a magnesium-zirconium intermediate alloy is added into an intermediate magnesium melt, a stirrer 4 in a stirring device is deeply inserted into one third of the height of the intermediate magnesium melt and is stirred for 1-3min, then the stirrer is positioned at the bottom of the intermediate magnesium melt and is stirred for 1-3min, and finally the stirrer is positioned at one third of the height of the intermediate magnesium melt and is stirred for 1-3min, so that the stirrer 4 is arranged to ensure that the whole intermediate magnesium melt rotates around from the bottom to the liquid level in a large range in order, zirconium element particles are ensured to be uniformly suspended in the intermediate magnesium melt, the zirconium element particles are prevented from sinking to the bottom, and the dissolving reaction process of zirconium and molten magnesium is accelerated; the zirconium element particles which have been sunk are re-melted in the intermediate magnesium melt, so that the zirconium yield is further improved, the grain refining effect is improved, and the production cost is reduced. The axial flow and the radial flow in each melt are more favorable for reaction mixing, and the invention also provides a sleeve or 4-6 baffle plates 2 in the first heating device 1, and 4-6 baffle plates 2 are evenly distributed on the inner surface of the first heating device 1, so that the arrangement can weaken horizontal co-rotating flow and obtain regular axial flow and radial flow.
Because solid inclusions and gas with the specific gravity being lighter than that of the alloy melt exist in the alloy melt, in order to further remove part of impurities in the alloy melt, the invention adds a solvent for refining to remove impurities, and then introduces refining gas to remove impurities through a gas conveying device, wherein the refining gas is argon or/and nitrogen, and the introduction time of the refining gas is 5-10 min. The preferred gas delivery device of the present invention has the structure: as shown in fig. 3 again, gas conveying device includes the gas tank, the desicator, guide arm 5, rotatory nozzle 6, the gas tank is connected with 5 one end of guide arm through the trachea, the other end of guide arm 5 is connected with rotatory nozzle 6, the desicator sets up on the trachea, the desicator is used for carrying out the drying to the gas that lets in, during the use, form the gas-liquid vortex of quick rotation deeply in the fit fuse-element through rotatory nozzle 6, produce a large amount of tiny bubbles, it is mingled with gaseous to get rid of at the floating in-process, reach the effect of degasification row sediment.
In conclusion, the invention has the following beneficial effects:
1. the alloying of the zirconium-free alloy ingot and the magnesium-zirconium intermediate alloy is respectively carried out, and the alloying temperature of the magnesium-zirconium intermediate alloy is increased to 780-800 ℃, so that the solubility of zirconium in the intermediate magnesium melt can be improved, the yield of zirconium is improved, and the production cost is reduced.
2. Stirring is carried out through a stirring device in the refining process, large-range axial and radial flow and small-area turbulence are formed in the molten magnesium melt, the intermediate magnesium melt and the alloy melt, heat transmission from the outer edge of each melt to the central part is enhanced, and element uniform mixing in each melt is promoted.
3. After the magnesium-zirconium intermediate alloy is added into the intermediate magnesium melt, a stirrer 4 in a stirring device extends into one third of the height of the intermediate magnesium melt and is stirred for 1-3min, then the stirrer is positioned at the bottom of the intermediate magnesium melt and is stirred for 1-3min, and finally the stirrer is positioned at one third of the height of the intermediate magnesium melt and is stirred for 1-3min, so that zirconium element particles which have settled at the bottom in the intermediate magnesium melt are re-melted in the intermediate magnesium melt, the yield of zirconium is further improved, the grain refining effect is improved, and the production cost is reduced.
4. The composite refining technology of firstly flux refining, then gas refining and finally standing sedimentation is adopted, so that sinking impurities, floating impurities and gas are effectively removed, the produced zirconium-containing magnesium alloy has the advantages of less impurities, good purification effect and high purity of the zirconium-containing magnesium alloy.
5. The stirring device and the gas conveying device are simple in structure, good in using effect, strong in implementability and convenient to manufacture, maintain and overhaul.
Example 1
A composite refining method of a zirconium-containing magnesium alloy comprises the following steps:
a. the first heating device 1 comprises a crucible, the size of the crucible is 500mm in inner diameter and 1000mm in depth, 212.67kg of magnesium ingot is added into the crucible after the crucible is electrified and preheated to 450 ℃, the magnesium ingot is Mg >99.80 wt%, and the first heating device 1 melts the magnesium ingot into molten magnesium melt;
b. stirring the molten magnesium melt by a stirring device, wherein a stirrer 4 is positioned at one third of the height of the molten magnesium melt, when the first heating device 1 is continuously heated to ensure that the temperature of the molten magnesium melt reaches 750 ℃, adding 1.50kg of zinc sheets and 20.83kg of magnesium-neodymium intermediate alloy preheated by a crucible into the molten magnesium melt, wherein the zinc sheets are Zn more than 99.95 wt%, and the magnesium-neodymium intermediate alloy is Mg-30Nd wt%, and continuously stirring for 3min by the stirring device under the condition of not damaging the liquid level of the melt to obtain an intermediate magnesium melt (Mg-Nd-Zn melt);
c. in the process of stirring the intermediate magnesium melt by a stirring device, when the crucible is continuously heated to enable the temperature of the intermediate magnesium melt to be 790 ℃, adding 15.00kg of magnesium-zirconium intermediate alloy preheated by the crucible into the intermediate magnesium melt, wherein the magnesium-zirconium intermediate alloy is Mg-25Zr wt.%, and after the magnesium-zirconium intermediate alloy is added into the intermediate magnesium melt, stirring for 2min by a stirrer 4 in the stirring device when the stirrer is deep into one third of the height of the intermediate magnesium melt, then stirring for 2min by positioning the stirrer 4 at the bottom of the intermediate magnesium melt, and finally stirring for 2min by positioning the stirrer 4 at one third of the height of the intermediate magnesium melt, thereby obtaining an alloy melt;
d. removing slag on the surface of the alloy melt;
e. after fracture detection is qualified, reducing the temperature of the alloy melt to 750 ℃, adding a refining flux RJ-5 into the alloy melt, and continuously stirring for 10min by using a stirring device;
f. the temperature of the alloy melt is continuously maintained at 750 ℃, argon for refining is added into the alloy melt through a gas conveying device, the purity of the argon is 99.999%, and the introducing time of the gas for refining is 8 min;
g. standing for 10min, further removing impurities by a gravity settling method, then cooling to a casting temperature, and carrying out subsequent deslagging, liquid transferring and pouring operations.
Blowing gas (CO) in the whole composite refining process2And 0.18% SF6) Each melt was protected.
The detection shows that the obtained zirconium-containing magnesium alloy comprises Mg-2.5Nd-0.6Zn-1.5Zr wt.%.
Claims (5)
1. A composite refining method of a zirconium-containing magnesium alloy is characterized by comprising the following steps:
a. adding a magnesium ingot into the first heating device (1), and melting the magnesium ingot into a molten magnesium melt by the first heating device (1);
b. stirring the molten magnesium melt by a stirring device, continuously heating by the first heating device (1) to ensure that alloy element ingots are added into the molten magnesium melt when the temperature of the molten magnesium melt reaches 740-760 ℃, and continuously stirring by the stirring device for a certain time to obtain an intermediate magnesium melt;
c. in the process of stirring the intermediate magnesium melt by the stirring device, when the first heating device (1) continues to heat the intermediate magnesium melt to 780-800 ℃, adding magnesium-zirconium intermediate alloy into the intermediate magnesium melt, and continuously stirring for a certain time by the stirring device to obtain an alloy melt;
d. removing floating slag on the surface of the alloy melt;
e. reducing the temperature of the alloy melt to 750-760 ℃, adding a flux for refining into the alloy melt, and continuously stirring for a certain time by using a stirring device;
f. the temperature of the alloy melt is maintained between 750 ℃ and 760 ℃, and gas for refining is added into the alloy melt through a gas conveying device;
g. the temperature of the alloy melt is reduced to the casting temperature;
the stirring device comprises a motor, a speed reducer, a connecting shaft (3) and a stirrer (4), wherein the stirrer (4) is an axial propelling stirrer, an output shaft of the motor is connected with the speed reducer, one end of the connecting shaft (3) is connected with the speed reducer, and the other end of the connecting shaft is connected with the stirrer (4); the gas conveying device comprises a gas tank, a dryer, a guide rod (5) and a rotary spray head (6), wherein the gas tank is connected with one end of the guide rod (5) through a gas pipe, the other end of the guide rod (5) is connected with the rotary spray head (6), and the dryer is arranged on the gas pipe;
in the step b, a stirrer (4) in the stirring device is deeply inserted into the molten magnesium melt for stirring, the stirrer (4) is positioned at one third of the height of the molten magnesium melt, the alloy element ingot is preheated by the second heating device and then added into the molten magnesium melt, and the stirring time of the stirring device is 3-5min after the alloy element ingot is added into the molten magnesium melt;
in the step c, the magnesium-zirconium intermediate alloy is preheated by the third heating device and then added into the intermediate magnesium melt, after the magnesium-zirconium intermediate alloy is added into the intermediate magnesium melt, a stirrer (4) in the stirring device extends into one third of the height of the intermediate magnesium melt and is stirred for 1-3min, then the stirrer (4) is positioned at the bottom of the intermediate magnesium melt and is stirred for 1-3min, and finally the stirrer (4) is positioned at one third of the height of the intermediate magnesium melt and is stirred for 1-3 min.
2. The composite refining method of a zirconium-containing magnesium alloy according to claim 1, wherein: in the step a, after the first heating device (1) is electrified and preheated to 400-.
3. The composite refining method of a zirconium-containing magnesium alloy according to claim 1, wherein: the first heating device (1) is internally provided with a sleeve or 4-6 baffles (2), and the 4-6 baffles (2) are evenly distributed on the inner surface of the first heating device (1).
4. The composite refining method of a zirconium-containing magnesium alloy according to claim 1, wherein: in the step e, a refining flux of RJ-5 is added into the alloy melt, and the stirring device continuously stirs for 10-15 min.
5. The composite refining method of a zirconium-containing magnesium alloy according to claim 1, wherein: in the step f, the refining gas is argon or/and nitrogen, and the refining gas is introduced for 5-10 min.
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