CN113444909B - Grain refinement method for large-size semi-continuous casting magnesium alloy ingot - Google Patents
Grain refinement method for large-size semi-continuous casting magnesium alloy ingot Download PDFInfo
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- C22C1/00—Making non-ferrous alloys
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Abstract
The invention provides a grain refining method for a large-size semi-continuous casting magnesium alloy ingot, which comprises the steps of feeding a Mg-Ti-Zr grain refining alloy wire to the middle part of a magnesium alloy melt through a wire feeding method in the solidification process of the magnesium alloy melt, wherein the alloy wire comprises 0.5-15% of Ti, 10-25% of Zr, less than 1% of unavoidable impurity elements and the balance of Mg. According to the invention, the distribution of the grain refining particles of the large-size magnesium alloy ingot is regulated and controlled by a wire feeding method, so that the temperature field distribution, the component distribution and the grain refiner distribution generate a synergistic effect, the precise regulation and control of the grain size in a macroscopic region are realized, the fine and macroscopically uniform grain size of the large-size magnesium alloy ingot is finally realized, the comprehensive mechanical property is improved, and the popularization and application of the large-size magnesium alloy ingot are facilitated.
Description
Technical Field
The invention belongs to the technical field of magnesium alloy materials, and particularly relates to a grain refining method for a large-size semi-continuous casting magnesium alloy ingot.
Background
The magnesium alloy is used as the lightest metal material for the structure, has the advantages of high specific strength, high specific stiffness, excellent shock absorption and noise reduction performance, good electromagnetic shielding performance, excellent machining performance, easy recovery and the like, can replace the traditional steel and aluminum alloy, and has wide application prospect in the fields of aviation, aerospace, automobiles and the like. The large-size magnesium alloy ingot can be used for producing and manufacturing large-size key components of equipment in the field of aerospace, the light weight effect is more remarkable, and the large-size magnesium alloy ingot has great application value and market prospect.
At present, large-size magnesium alloy ingots are difficult to manufacture, and have the problems of complex temperature field and components, so that the internal and external cooling speeds in the material solidification process are uneven, the phenomena of uneven internal and external crystal grain sizes, unstable mechanical properties, easiness in cracking of the ingots and the like of the obtained large-size magnesium alloy ingots are caused, and the product quality of the ingots is seriously influenced. Therefore, a method for regulating and controlling the grain size is found, the small and macroscopically uniform crystal grains of the cast ingot are ensured, and the method has great significance for the production and application of large-size magnesium alloy cast ingots.
Disclosure of Invention
The invention aims to overcome the problems of uneven grain size and large grains of the existing large-size magnesium alloy ingot, provides a grain refining method for the large-size semi-continuous casting magnesium alloy ingot, and realizes uniform and fine grain size of the prepared magnesium alloy product.
The technical scheme provided by the invention is as follows:
a grain refining method for large-size semi-continuous casting magnesium alloy ingots comprises the following steps: in the process of solidifying the magnesium alloy melt, feeding Mg-Ti-Zr grain refined alloy wires to the middle part of the magnesium alloy melt through a wire feeding method, wherein the alloy wires comprise 0.5-15% of Ti, 10-25% of Zr, less than 1% of inevitable impurity elements and the balance of Mg.
Specifically, the grain refining method for the large-size semi-continuous casting magnesium alloy ingot comprises the following steps:
s1, batching: weighing raw materials according to the components of the magnesium alloy ingot;
s2, smelting: putting the weighed raw materials into a smelting furnace for smelting, and transferring the magnesium alloy melt to a refining furnace after smelting is finished;
s3, refining: adding a magnesium alloy refining agent into the refining furnace, and transferring the magnesium alloy melt to a holding furnace after refining;
s4, preliminary refinement and heat preservation: adding a grain refiner into a holding furnace, standing and holding;
s5, secondary refining and solidification: and finally transferring the magnesium alloy melt into a crystallizer for solidification, feeding Mg-Ti-Zr grain refined alloy wires to the middle part of the magnesium alloy melt for secondary local refinement, and drawing blanks in the solidification process to finally obtain the semi-continuous casting magnesium alloy ingot.
The grain refining method for the large-size semi-continuous casting magnesium alloy ingot has the following beneficial effects:
(1) the invention provides a grain refining method for a large-size semi-continuous casting magnesium alloy ingot, which adopts Mg-Ti-Zr grain refining alloy wires as grain refiners for local adjustment, aims at the problem that the difference between the central grain size and the edge grain size of the large-size semi-continuous casting high-rare earth magnesium alloy ingot is large at present, directionally refines grains in a billet and integrally improves the quality of the magnesium alloy ingot.
(2) The invention provides a grain refining method for large-size semi-continuous casting magnesium alloy ingots, which adjusts the wire feeding quantity according to the size of a target billet ingot and effectively controls the grain refining effect.
(3) According to the method for refining the crystal grains of the large-size semi-continuous casting magnesium alloy ingot, the distribution of the refined crystal grains of the large-size magnesium alloy ingot is regulated and controlled through a wire feeding method, so that the temperature field distribution, the component distribution and the distribution of a crystal grain refiner generate a synergistic effect, the precise regulation and control of the crystal grain size in a macroscopic region are realized, the fine crystal grains and the macroscopic uniformity of the crystal grain size of the large-size magnesium alloy ingot are finally realized, the comprehensive mechanical property of the large-size magnesium alloy ingot is improved, and the popularization and the application of the large-size magnesium alloy ingot are facilitated.
Drawings
FIG. 1 is an internal metallographic view of a large-gauge semi-continuously cast high rare earth magnesium alloy ingot according to example 2;
FIG. 2 is an external metallographic picture of a large-gauge semi-continuously cast high rare earth magnesium alloy ingot according to example 2.
Detailed Description
The features and advantages of the present invention will become more apparent and appreciated from the following detailed description of the invention.
The word "exemplary" is used exclusively herein to mean "serving as an example, embodiment, or illustration. Any embodiment described herein as "exemplary" is not necessarily to be construed as preferred or advantageous over other embodiments. While the various aspects of the embodiments are presented in drawings, the drawings are not necessarily drawn to scale unless specifically indicated.
The invention provides a grain refining method for a large-size semi-continuous casting magnesium alloy ingot, which comprises the following steps:
in the process of solidifying the magnesium alloy melt, feeding Mg-Ti-Zr grain refined alloy wires to the middle part of the magnesium alloy melt through a wire feeding method, wherein the alloy wires comprise 0.5-15% of Ti, 10-25% of Zr, less than 1% of inevitable impurity elements and the balance of Mg; preferably, the alloy wire comprises 5-15% of Ti, 15-25% of Zr, less than 1% of unavoidable impurity elements and the balance of Mg.
In the invention, an Mg-Ti-Zr grain refining alloy wire is used as a grain refiner at the stage, Zr and Ti are in a close hexagonal structure with the same genus as Mg, the lattice constant (a is 0.295nm, c is 0.468nm) of alpha-Ti and the lattice constant (a is 0.323nm, c is 0.514) of alpha-Zr are close to that of Mg (a is 0.321nm, c is 0.521nm), and the alloy wire has a good coherent relation with Mg, wherein the mismatching degree between Zr and Mg is only 0.9 percent, and both can be used as high-quality heterogeneous nucleation cores of Mg from the aspect of crystallography. Meanwhile, Ti, Zr and Mg are peritectic reaction, under the solute distribution effect, the actual temperature of the front edge of a solid/liquid interface in solidification is lower than the equilibrium solidification temperature of a liquid phase, so that the component supercooling effect is generated, in a component supercooling region, the diffusion speed of solute atoms is slowed down along with the reduction of the temperature, and the grain Growth rate is reduced, so that the grain refining mechanism is called a Growth inhibition mechanism, and is quantified as a Growth inhibition factor (GRF). The GRF value of Ti is the largest known at present, and is calculated by research to be 59500, and the GRF value of zirconium is 3829, so that theoretically the Mg-Ti-Zr grain refiner has better grain refining effect than the traditional Mg-Zr intermediate alloy. However, Ti and Mg are known to have extremely low solid solubility, and are difficult to blend. Through research, the inventor adds Zr and Ti into Mg together, solves the problem that Ti and Mg are difficult to blend, and effectively improves the grain refining effect.
The feeding wire is directionally fed into the middle part of the magnesium alloy melt in the solidification process of the magnesium alloy melt, so that the central part of the large-size semi-continuous casting high rare earth magnesium alloy billet is directionally refined by the high-quality grain refiner, the effect of uniform sizes of the inner grain and the outer grain of the large-size magnesium alloy billet is achieved, and the problem that the size of the central grain of the semi-continuous casting magnesium alloy billet is far larger than that of the outer part of the billet in the traditional process is solved. In the traditional semi-continuous casting process by the wire feeding method, the wire feeding position is usually a liquid guide pipe of a heat-preservation standing furnace and a crystallizer, and the aim is to efficiently add a grain refiner and realize the grain refinement of the whole billet. However, the method cannot solve the problem that the central grain size of the large-size semi-continuous casting billet is far larger than the edge grain size, and has obvious defects compared with the prior art.
In the invention, the semi-continuous casting magnesium alloy ingot comprises the chemical components of 7-15% of Gd, 0-7% of Y, 0-4% of Nd, 0-1.5% of Zn, 0.1-0.6% of Zr, 0-0.2% of Ti, less than 1% of unavoidable impurity elements and the balance of Mg; the diameter of the billet is 150-500 mm. Preferably, the chemical composition of the semi-continuous casting magnesium alloy ingot does not contain Al.
In the invention, the grain refining method for the large-size semi-continuous casting magnesium alloy ingot specifically comprises the following steps:
s1, batching: weighing raw materials according to the components of the magnesium alloy ingot;
s2, smelting: putting the weighed raw materials into a smelting furnace for smelting, and transferring the magnesium alloy melt to a refining furnace after smelting is finished;
s3, refining: adding a magnesium alloy refining agent into the refining furnace, and transferring the magnesium alloy melt to a holding furnace after refining;
s4, preliminary refinement and heat preservation: adding a grain refiner into a holding furnace, standing and holding;
s5, secondary refining and solidification: and finally transferring the magnesium alloy melt into a crystallizer for solidification, feeding Mg-Ti-Zr grain refined alloy wires to the middle part of the magnesium alloy melt for secondary local refinement, and drawing blanks in the solidification process to finally obtain the semi-continuous casting magnesium alloy ingot.
Further, in step S4, the grain refiner is an Mg-Zr intermediate alloy or an Mg-Ti-Zr intermediate alloy, wherein the Mg-Zr intermediate alloy contains 10 to 30% by mass of Zr, less than 1% of unavoidable impurity elements, and the balance Mg;
the Mg-Ti-Zr intermediate alloy comprises 0.5-15% of Ti, 10-25% of Zr, less than 1% of unavoidable impurity elements and the balance of Mg by mass percent; preferably, the alloy wire comprises 5-15% of Ti, 15-25% of Zr, less than 1% of unavoidable impurity elements and the balance of Mg.
In step S4, the temperature is kept at 720 +/-30 ℃, and the mixture is kept stand for 5-30 min.
Further, in the step S5, the solidification temperature is 700 +/-30 ℃, the throwing speed is 10-50 mm/min, the liquid level height of the crystallizer is 30-150 mm, and the diameter of the crystallizer is 150-500 mm.
In the step S5, the wire feeding area is located in the middle of the magnesium alloy melt, and when the size of the billet is 150-250 mm, only one wire feeder is needed to feed a grain refining alloy wire in the middle; when the size of the billet is 250-500 mm, two wire feeding machines are required to work together, two grain refined alloy wires are fed at the same speed, and the wire feeding positions of the two devices are 10-40 mm apart.
In the step S5, the wire feeding speed is consistent with the blank drawing speed and is 10-50 mm/min;
in step S5, the diameter of the grain refining alloy wire is 0.2-5 mm, and the total wire feeding length is consistent with the billet length.
Further, steps S2 to S5 are all operated under an inert atmosphere.
Examples
Example 1
A large-size semi-continuous casting high rare earth magnesium alloy ingot is 200mm in diameter and 1m in length, and comprises the following components in percentage by mass: 15% of Gd; zn is 1 percent; zr is 0.5%; the balance being Mg and unavoidable impurity elements (< 1%).
A preparation method of a large-size semi-continuous casting high rare earth magnesium alloy ingot comprises the following steps:
s1, batching according to the size of the magnesium ingot and the alloy burning loss condition, and preheating the intermediate alloy;
s2, adding magnesium ingots into a smelting furnace, adding various intermediate alloys at required temperature, stirring until the intermediate alloys are completely molten, and transferring the magnesium melt to a refining furnace after the smelting is finished;
s3, raising the temperature of the melt to 710 ℃, selecting JDMJ as a refining agent, refining for 5min, skimming surface scum after refining, and transferring the magnesium melt to a holding furnace after refining;
s4, standing and preserving heat in a heat preservation furnace, adding 10kg of Mg-30Zr intermediate alloy, keeping the heat preservation temperature at 710 ℃, and standing for 15 min;
s5, transferring the magnesium alloy melt into a crystallizer for solidification, feeding Mg-Ti-Zr alloy wires to the middle part of the melt, wherein the solidification temperature is 680 ℃, the casting speed is 30mm/min, the liquid level height of the crystallizer is 1000mm, the wire feeding area is the center of a magnesium alloy ingot, 1 wire feeder works, the wire feeding speed is 30mm/min, the diameter of the Mg-Zr alloy wires is 2mm, the mass fraction of Ti is 10%, the mass fraction of Zr is 25%, and the balance is Mg; the size of the selected crystallizer is 200mm, and finally the semi-continuous casting magnesium alloy ingot is prepared.
The magnesium alloy ingot is detected to have fine grains and uniform macro-size of the grains, the size of the grains in the ingot is about 51 mu m, and the average size of the grains at the edge part is about 42 mu m.
Example 2
A large-size semi-continuous casting high rare earth magnesium alloy ingot is 300mm in diameter and 1m in length, and comprises the following components in percentage by mass: 10% of Gd; zr is 0.4%; ti is 0.1%; the balance being Mg and unavoidable impurity elements (< 1%).
A preparation method of a large-size semi-continuous casting high rare earth magnesium alloy ingot comprises the following steps:
s1, batching according to the size of the magnesium ingot and the alloy burning loss condition, and preheating the intermediate alloy;
s2, adding magnesium ingots into a smelting furnace, adding various intermediate alloys at required temperature, stirring until the intermediate alloys are completely molten, and transferring the magnesium melt to a refining furnace after the smelting is finished;
s3, raising the temperature of the melt to 710 ℃, selecting JDMJ as a refining agent, refining for 5min, skimming the surface scum after the refining is finished, and transferring the magnesium melt to a holding furnace after the refining is finished;
s4, standing and preserving heat in a heat preservation furnace, adding 15kg of Mg-30Zr intermediate alloy, keeping the temperature at 710 ℃, and standing for 15 min;
s5, transferring the magnesium alloy melt into a crystallizer for solidification, feeding Mg-Ti-Zr alloy wires to the middle part of the melt, wherein the solidification temperature is 680 ℃, the casting speed is 30mm/min, the liquid level height of the crystallizer is 1000mm, the wire feeding area is the center of a magnesium alloy cast ingot, two wire feeding machines work together, the wire feeding positions of the two devices are separated by 10mm, the wire feeding speed is 30mm/min, the diameter of the Mg-Ti-Zr alloy wires is 3mm, and the mass fraction of each element of the wire is Zr: 20%, Ti: 10 percent, and the size of the selected crystallizer is 300mm, and finally the semi-continuous casting magnesium alloy ingot is prepared.
The magnesium alloy ingot is detected to have fine grains and uniform macroscopic size of the grains, the size of the grains in the ingot is about 59 mu m, the average size of the grains at the edge part is about 47 mu m, and the metallographic pictures are shown in figure 1 and figure 2.
Example 3
A large-size semi-continuous casting high rare earth magnesium alloy ingot is 300mm in diameter and 1m in length, and comprises the following components in percentage by mass: gd is 9 percent; y is 4%; zn is 1 percent; zr is 0.4%; the balance being Mg and unavoidable impurity elements (< 1%).
A preparation method of a large-size semi-continuous casting high rare earth magnesium alloy ingot comprises the following steps:
s1, batching according to the size of the magnesium ingot and the alloy burning loss condition, and preheating the intermediate alloy;
s2, adding magnesium ingots into a smelting furnace, adding various intermediate alloys at required temperature, stirring until the intermediate alloys are completely molten, and transferring the magnesium melt to a refining furnace after the smelting is finished;
s3, raising the temperature of the melt to 710 ℃, selecting JDMJ as a refining agent, refining for 5min, skimming the surface scum after the refining is finished, and transferring the magnesium melt to a holding furnace after the refining is finished;
s3, raising the temperature of the melt to 710 ℃, selecting JDMJ as a refining agent, refining for 5min, skimming surface scum after refining, and transferring the magnesium melt to a holding furnace after refining;
s4, standing and preserving heat in a heat preservation furnace, adding 15kg of Mg-30Zr intermediate alloy, keeping the temperature at 710 ℃, and standing for 15 min;
s5, transferring the magnesium alloy melt into a crystallizer for solidification, feeding Mg-Ti-Zr alloy wires to the middle part of the melt, wherein the solidification temperature is 680 ℃, the casting speed is 30mm/min, the liquid level height of the crystallizer is 100mm, the wire feeding area is the center of a magnesium alloy cast ingot, two wire feeding machines work together, the wire feeding positions of the two devices are separated by 10mm, the wire feeding speed is 30mm/min, the diameter of the Mg-Ti-Zr alloy wires is 3mm, and the mass fraction of each element of the wire is Zr: 25%, Ti: 15 percent, and the size of the selected crystallizer is 300mm, and finally the semi-continuous casting magnesium alloy ingot is prepared.
The magnesium alloy ingot is detected to have fine grains and uniform macro-size of the grains, the size of the grains in the ingot is about 73 mu m, and the average size of the grains at the edge part is about 61 mu m.
Comparative example 1
This comparative example is that of example 2, differing from example 2 only in that no wire feed controls the grain refinement process.
Through detection, the grain size of the magnesium alloy ingot obtained by the comparative example is about 93 μm at the center position, about 42 μm at the edge position, and the grain size difference is large. Example 2 has finer grains and closer grain sizes at the center and edge than the comparative example. The comparison example proves that the invention successfully enables the temperature field distribution, the component distribution and the grain refiner distribution in the magnesium ingot cooling process to generate synergistic effect based on the regulation and control of the grain refined particle distribution of the large-size magnesium alloy ingot by the wire feeding method, realizes the precise regulation and control of the grain size in the macroscopic region, and is beneficial to improving the comprehensive mechanical property of the large-size magnesium alloy ingot.
The invention has been described in detail with reference to specific embodiments and illustrative examples, but the description is not intended to be construed in a limiting sense. Those skilled in the art will appreciate that various equivalent substitutions, modifications or improvements may be made to the technical solution of the present invention and its embodiments without departing from the spirit and scope of the present invention, which fall within the scope of the present invention. The scope of the invention is defined by the appended claims.
Those skilled in the art will appreciate that those matters not described in detail in the present specification are well known in the art.
Claims (5)
1. A grain refinement method for large-size semi-continuous casting magnesium alloy ingots is characterized in that in the solidification process of a magnesium alloy melt, a Mg-Ti-Zr grain refinement alloy wire is fed to the middle part of the magnesium alloy melt through a wire feeding method, the alloy wire comprises the chemical components of 0.5-15% of Ti, 10-25% of Zr, less than 1% of unavoidable impurity elements and the balance of Mg;
the method specifically comprises the following steps:
s1, batching: weighing raw materials according to the components of the magnesium alloy ingot;
s2, smelting: putting the weighed raw materials into a smelting furnace for smelting, and transferring the magnesium alloy melt to a refining furnace after smelting is finished;
s3, refining: adding a magnesium alloy refining agent into the refining furnace, and transferring the magnesium alloy melt to a holding furnace after refining;
s4, preliminary refinement and heat preservation: adding a grain refiner into a heat preservation furnace, standing and preserving heat, wherein the heat preservation temperature is 720 +/-30 ℃, and standing for 5-30 min;
s5, secondary refining and solidification: finally, transferring the magnesium alloy melt into a crystallizer for solidification, wherein the solidification temperature is 700 +/-30 ℃, the blank drawing speed is 10-50 mm/min, the liquid level height of the crystallizer is 30-150 mm, the diameter of the crystallizer is 150-500 mm, and Mg-Ti-Zr grain refined alloy wires are fed to the middle part of the magnesium alloy melt for secondary local refinement, a wire feeding area is positioned at the middle part of the magnesium alloy melt, and when the size of a billet is 150-250 mm, only one grain refined alloy wire is fed to the middle part; and when the size of the billet is 250-500 mm, only feeding two grain refined alloy wires at the middle part at the same speed, wherein the distance between the two wire feeding positions is 10-40 mm, and pulling in the solidification process to finally obtain the semi-continuous casting magnesium alloy ingot.
2. The method for refining the crystal grains of the large-size semi-continuous casting magnesium alloy ingot according to claim 1, wherein the semi-continuous casting magnesium alloy ingot comprises 7-15% of Gd, 0-7% of Y, 0-4% of Nd, 0-1.5% of Zn, 0.1-0.6% of Zr, 0-0.2% of Ti, less than 1% of unavoidable impurity elements, and the balance of Mg.
3. The method for grain refinement of a large-gauge semi-continuously cast magnesium alloy ingot according to claim 1, wherein in step S4, the grain refiner is a Mg-Zr master alloy or a Mg-Ti-Zr master alloy.
4. The method for grain refinement of a large-gauge semi-continuously cast magnesium alloy ingot according to claim 1, wherein in step S5, the wire feeding speed is in accordance with the withdrawal speed.
5. The method for grain refinement of a large-gauge semi-continuously cast magnesium alloy ingot according to claim 1, wherein in step S5, the diameter of the grain refined alloy wire is 0.2 to 5mm, and the total length of the wire feed is in accordance with the length of the ingot.
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